# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_CuBr2Pyz100K _database_code_depnum_ccdc_archive 'CCDC 925063' #TrackingRef '17871_web_deposit_cif_file_0_SaulH.Lapidus_1361228198.CuBr2(pyz)_100K.cif' #=========================================================================== # # The submitted manuscript has been created by UChicago Argonne, LLC, # Operator of Argonne National Laboratory ("Argonne"). Argonne, a U.S. # Department of Energy Office of Science laboratory, is operated under # Contract No. DE-AC02-06CH11357. The U.S. Government retains for itself, # and others acting on its behalf, a paid-up nonexclusive, irrevocable # worldwide license in said article to reproduce, prepare derivative works, # distribute copies to the public, and perform publicly and display # publicly, by or on behalf of the Government. #=========================================================================== _audit_creation_method 'manual editing of SHELXL-97 cif file' _chemical_name_systematic ; catena(bis(\m~2~-bromo)-(\m~2~-pyrazine-N,N')-copper(II)) ; _chemical_name_common ; Copper(II) difluoride pyrazine ; _chemical_melting_point ? _chemical_formula_moiety 'Cu 2+, 2(Br 1-), C4 H4 N2' _chemical_formula_sum 'C4 H4 Br2 Cu N2' _chemical_formula_weight 303.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_space_group_name_Hall '-C 2y' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 12.3718(5) _cell_length_b 6.8551(2) _cell_length_c 3.87760(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.9450(10) _cell_angle_gamma 90.00 _cell_volume 327.090(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3382 _cell_measurement_theta_min 3.311 _cell_measurement_theta_max 31.526 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 282 _exptl_absorpt_coefficient_mu 15.450 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.033 _exptl_absorpt_correction_T_max 0.295 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space by a combination of five sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.000 cm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '3-circle goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_reflns_number 3600 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0126 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 31.53 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 31.53 _diffrn_measured_fraction_theta_full 0.997 _reflns_number_total 591 _reflns_number_gt 586 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II v.2.2 (Bruker, 2007)' _computing_cell_refinement 'APEX II v.2.2 (Bruker, 2007)' _computing_data_reduction 'APEX II v.2.2 (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 3.1a (Crystal Impact, 2005)' _computing_publication_material 'SHELXTL (Bruker, 2006)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+0.6240P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 591 _refine_ls_number_parameters 25 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0153 _refine_ls_R_factor_gt 0.0151 _refine_ls_wR_factor_ref 0.0397 _refine_ls_wR_factor_gt 0.0395 _refine_ls_goodness_of_fit_ref 1.216 _refine_ls_restrained_S_all 1.216 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.726 _refine_diff_density_min -0.992 _refine_diff_density_rms 0.132 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.653408(15) 0.0000 0.44622(5) 0.00722(7) Uani 1 2 d S . . Cu1 Cu 0.5000 0.0000 0.0000 0.00700(9) Uani 1 4 d S . . N1 N 0.5000 0.2967(3) 0.0000 0.0075(3) Uani 1 2 d S . . C1 C 0.41052(12) 0.3986(2) 0.0541(4) 0.0086(2) Uani 1 1 d . . . H1 H 0.3460 0.3307 0.0931 0.010 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.00770(11) 0.00565(11) 0.00834(11) 0.000 0.00089(7) 0.000 Cu1 0.00822(16) 0.00194(16) 0.01051(17) 0.000 -0.00065(12) 0.000 N1 0.0092(7) 0.0041(7) 0.0093(7) 0.000 0.0007(6) 0.000 C1 0.0090(6) 0.0051(6) 0.0120(6) 0.0003(5) 0.0029(5) -0.0002(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Cu1 2.4322(2) . ? Cu1 N1 2.0336(18) 5_655 ? Cu1 N1 2.0336(18) . ? Cu1 Br1 2.4322(2) 5_655 ? N1 C1 1.3437(17) 2_655 ? N1 C1 1.3437(17) . ? C1 C1 1.391(3) 6_565 ? C1 H1 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 180.0 5_655 . ? N1 Cu1 Br1 90.0 5_655 5_655 ? N1 Cu1 Br1 90.0 . 5_655 ? N1 Cu1 Br1 90.0 5_655 . ? N1 Cu1 Br1 90.0 . . ? Br1 Cu1 Br1 179.999(1) 5_655 . ? C1 N1 C1 117.35(18) 2_655 . ? C1 N1 Cu1 121.32(9) 2_655 . ? C1 N1 Cu1 121.32(9) . . ? N1 C1 C1 121.32(9) . 6_565 ? N1 C1 H1 119.3 . . ? C1 C1 H1 119.3 6_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Br1 Cu1 N1 C1 -124.49(8) 5_655 . . 2_655 ? Br1 Cu1 N1 C1 55.51(8) . . . 2_655 ? Br1 Cu1 N1 C1 55.51(8) 5_655 . . . ? Br1 Cu1 N1 C1 -124.49(8) . . . . ? C1 N1 C1 C1 0.0 2_655 . . 6_565 ? Cu1 N1 C1 C1 180.0 . . . 6_565 ? data_CuCl2Pyz100K _database_code_depnum_ccdc_archive 'CCDC 925064' #TrackingRef '17872_web_deposit_cif_file_1_SaulH.Lapidus_1361228198.CuCl2(pyz)_100K.cif' #=========================================================================== # # The submitted manuscript has been created by UChicago Argonne, LLC, # Operator of Argonne National Laboratory ("Argonne"). Argonne, a U.S. # Department of Energy Office of Science laboratory, is operated under # Contract No. DE-AC02-06CH11357. The U.S. Government retains for itself, # and others acting on its behalf, a paid-up nonexclusive, irrevocable # worldwide license in said article to reproduce, prepare derivative works, # distribute copies to the public, and perform publicly and display # publicly, by or on behalf of the Government. #=========================================================================== _audit_creation_method 'manual editing of SHELXL-97 cif file' _chemical_name_systematic ; catena(bis(\m~2~-chloro)-(\m~2~-pyrazine-N,N')-copper(II)) ; _chemical_name_common ; Copper(II) dichloride pyrazine ; _chemical_melting_point ? _chemical_formula_moiety 'Cu 2+, 2(Cl 1-), C4 H4 N2' _chemical_formula_sum 'C4 H4 Cl2 Cu N2' _chemical_formula_weight 214.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_space_group_name_Hall '-C 2y' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 11.9223(4) _cell_length_b 6.8500(2) _cell_length_c 3.67350(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.6560(10) _cell_angle_gamma 90.00 _cell_volume 298.546(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2809 _cell_measurement_theta_min 2.966 _cell_measurement_theta_max 31.500 _exptl_crystal_description rod _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.386 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 210 _exptl_absorpt_coefficient_mu 4.437 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6146 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space by a combination of five sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.000 cm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '3-circle goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_reflns_number 3122 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_sigmaI/netI 0.0105 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 31.50 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.996 _reflns_number_total 536 _reflns_number_gt 535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II v.2.2 (Bruker, 2007)' _computing_cell_refinement 'APEX II v.2.2 (Bruker, 2007)' _computing_data_reduction 'APEX II v.2.2 (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 3.1a (Crystal Impact, 2005)' _computing_publication_material 'SHELXTL (Bruker, 2006)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0173P)^2^+0.4203P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 536 _refine_ls_number_parameters 25 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0151 _refine_ls_R_factor_gt 0.0151 _refine_ls_wR_factor_ref 0.0398 _refine_ls_wR_factor_gt 0.0398 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.649 _refine_diff_density_min -0.255 _refine_diff_density_rms 0.079 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.0000 0.0000 0.00842(8) Uani 1 4 d S . . Cl1 Cl 0.64915(3) 0.0000 0.44238(9) 0.00965(9) Uani 1 2 d S . . N1 N 0.5000 0.29681(19) 0.0000 0.0089(2) Uani 1 2 d S . . C1 C 0.40792(9) 0.39847(15) 0.0663(3) 0.00985(19) Uani 1 1 d . . . H1 H 0.3415 0.3304 0.1142 0.012 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01041(13) 0.00378(12) 0.01080(13) 0.000 -0.00043(9) 0.000 Cl1 0.01048(16) 0.00776(16) 0.01061(16) 0.000 0.00060(12) 0.000 N1 0.0109(5) 0.0060(5) 0.0098(5) 0.000 0.0011(4) 0.000 C1 0.0109(4) 0.0066(4) 0.0122(4) 0.0001(3) 0.0016(3) -0.0004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.0332(13) . ? Cu1 N1 2.0332(13) 5_655 ? Cu1 Cl1 2.2876(4) 5_655 ? Cu1 Cl1 2.2876(4) . ? N1 C1 1.3425(13) 2_655 ? N1 C1 1.3425(13) . ? C1 C1 1.391(2) 6_565 ? C1 H1 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 180.0 . 5_655 ? N1 Cu1 Cl1 90.0 . 5_655 ? N1 Cu1 Cl1 90.0 5_655 5_655 ? N1 Cu1 Cl1 90.0 . . ? N1 Cu1 Cl1 90.0 5_655 . ? Cl1 Cu1 Cl1 180.0 5_655 . ? C1 N1 C1 117.51(13) 2_655 . ? C1 N1 Cu1 121.25(7) 2_655 . ? C1 N1 Cu1 121.25(7) . . ? N1 C1 C1 121.25(7) . 6_565 ? N1 C1 H1 119.4 . . ? C1 C1 H1 119.4 6_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Cu1 N1 C1 -122.82(5) 5_655 . . 2_655 ? Cl1 Cu1 N1 C1 57.18(5) . . . 2_655 ? Cl1 Cu1 N1 C1 57.18(5) 5_655 . . . ? Cl1 Cu1 N1 C1 -122.82(5) . . . . ? C1 N1 C1 C1 0.0 2_655 . . 6_565 ? Cu1 N1 C1 C1 179.999(1) . . . 6_565 ? data_CuCl2Pyz300K _database_code_depnum_ccdc_archive 'CCDC 925065' #TrackingRef '17873_web_deposit_cif_file_2_SaulH.Lapidus_1361228198.CuCl2(pyz)_300K.cif' #=========================================================================== # # The submitted manuscript has been created by UChicago Argonne, LLC, # Operator of Argonne National Laboratory ("Argonne"). Argonne, a U.S. # Department of Energy Office of Science laboratory, is operated under # Contract No. DE-AC02-06CH11357. The U.S. Government retains for itself, # and others acting on its behalf, a paid-up nonexclusive, irrevocable # worldwide license in said article to reproduce, prepare derivative works, # distribute copies to the public, and perform publicly and display # publicly, by or on behalf of the Government. #=========================================================================== _audit_creation_method 'manual editing of SHELXL-97 cif file' _chemical_name_systematic ; catena(bis(\m~2~-chloro)-(\m~2~-pyrazine-N,N')-copper(II)) ; _chemical_name_common ; Copper(II) dichloride pyrazine ; _chemical_melting_point ? _chemical_formula_moiety 'Cu 2+, 2(Cl 1-), C4 H4 N2' _chemical_formula_sum 'C4 H4 Cl2 Cu N2' _chemical_formula_weight 214.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_space_group_name_Hall '-C 2y' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 11.9927(3) _cell_length_b 6.85570(10) _cell_length_c 3.70700(10) _cell_angle_alpha 90.00 _cell_angle_beta 95.9350(10) _cell_angle_gamma 90.00 _cell_volume 303.150(12) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 2937 _cell_measurement_theta_min 3.416 _cell_measurement_theta_max 31.655 _exptl_crystal_description rod _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 210 _exptl_absorpt_coefficient_mu 4.370 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6325 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space by a combination of five sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.000 cm. ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '3-circle goniometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_reflns_number 3362 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.0098 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 31.66 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 31.66 _diffrn_measured_fraction_theta_full 0.998 _reflns_number_total 547 _reflns_number_gt 541 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II v.2.2 (Bruker, 2007)' _computing_cell_refinement 'APEX II v.2.2 (Bruker, 2007)' _computing_data_reduction 'APEX II v.2.2 (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond 3.1a (Crystal Impact, 2005)' _computing_publication_material 'SHELXTL (Bruker, 2006)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.2521P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 547 _refine_ls_number_parameters 25 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0162 _refine_ls_R_factor_gt 0.0160 _refine_ls_wR_factor_ref 0.0451 _refine_ls_wR_factor_gt 0.0450 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.149 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.522 _refine_diff_density_min -0.207 _refine_diff_density_rms 0.073 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.5000 0.0000 0.0000 0.01900(9) Uani 1 4 d S . . Cl1 Cl 0.64858(3) 0.0000 0.43966(10) 0.02131(10) Uani 1 2 d S . . N1 N 0.5000 0.29721(19) 0.0000 0.0182(2) Uani 1 2 d S . . C1 C 0.40862(10) 0.39876(16) 0.0633(3) 0.0205(2) Uani 1 1 d . . . H1 H 0.3439 0.3323 0.1081 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.02247(15) 0.00838(13) 0.02533(15) 0.000 -0.00148(10) 0.000 Cl1 0.02175(18) 0.01834(18) 0.02353(18) 0.000 0.00088(13) 0.000 N1 0.0210(6) 0.0105(5) 0.0229(6) 0.000 0.0023(5) 0.000 C1 0.0203(5) 0.0121(5) 0.0295(5) 0.0005(4) 0.0050(4) -0.0010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.0376(13) . ? Cu1 Cl1 2.2871(4) . ? N1 C1 1.3394(13) . ? C1 C1 1.388(2) 6_565 ? C1 H1 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N1 180.0 5_655 . ? N1 Cu1 Cl1 90.0 5_655 5_655 ? N1 Cu1 Cl1 90.0 . 5_655 ? N1 Cu1 Cl1 90.0 5_655 . ? N1 Cu1 Cl1 90.0 . . ? Cl1 Cu1 Cl1 180.0 5_655 . ? C1 N1 C1 117.36(13) 2_655 . ? C1 N1 Cu1 121.32(7) 2_655 . ? C1 N1 Cu1 121.32(7) . . ? N1 C1 C1 121.32(7) . 6_565 ? N1 C1 H1 119.3 . . ? C1 C1 H1 119.3 6_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl1 Cu1 N1 C1 -123.10(6) 5_655 . . 2_655 ? Cl1 Cu1 N1 C1 56.90(6) . . . 2_655 ? Cl1 Cu1 N1 C1 56.90(6) 5_655 . . . ? Cl1 Cu1 N1 C1 -123.10(6) . . . . ? C1 N1 C1 C1 0.0 2_655 . . 6_565 ? Cu1 N1 C1 C1 180.0 . . . 6_565 ? data_CuF2(44bipy)_100K _database_code_depnum_ccdc_archive 'CCDC 925066' #TrackingRef 'web_deposit_cif_file_3_SaulH.Lapidus_1361228198.CuF2(44bipy)_100K_pub.cif' # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C10 H8 Cu F2 N2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H8 Cu F2 N2' _chemical_formula_weight 257.73 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_length_neutron # include if applicable ? ? ? ? ? ? #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 2/m' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,-z 3 -x,-y,-z 4 x,-y,z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,z _cell_length_a 10.57016(13) _cell_length_b 11.145808(88) _cell_length_c 3.507797(63) _cell_angle_alpha 90 _cell_angle_beta 96.6254(12) _cell_angle_gamma 90 _cell_volume 410.504(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; capillary ; _pd_spec_mount_mode transmission # options are 'reflection' # or 'transmission' _pd_spec_shape cylinder # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? # include if applicable _exptl_absorpt_correction_type ? # include if applicable _exptl_absorpt_process_details ? # include if applicable _exptl_absorpt_correction_T_min ? # include if applicable _exptl_absorpt_correction_T_max ? # include if applicable #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; 11-BM, APS, Argonne National Lab ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 100 _diffrn_source synchrotron _diffrn_source_target ? _diffrn_source_type ? _diffrn_radiation_type synchrotron _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. _diffrn_radiation_wavelength 0.413920 _diffrn_radiation_monochromator 'Si(111) channel cut' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 29201 _pd_meas_2theta_range_min 2.0 _pd_meas_2theta_range_max 31.2 _pd_meas_2theta_range_inc 0.001 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; Molecules are defined as rigid bodies using the z-matrix function implemented in TOPAS. ; # The next three items are given as text. _pd_proc_ls_profile_function ; Simple_Axial_model function with Rp=9999,Rs=1000 in TOPAS ; _pd_proc_ls_background_function ; 2 Pearson-Voight peaks and Chebyshev polynomial with 10 coefficients ; _pd_proc_ls_pref_orient_corr ; none ; _pd_proc_ls_prof_R_factor 0.08244 # 8.244(%) _pd_proc_ls_prof_wR_factor 0.10724 # 10.724(%) _pd_proc_ls_prof_wR_expected 0.05432 # 5.432(%) _refine_ls_R_I_factor ? _refine_ls_R_Fsqd_factor ? _refine_ls_R_factor_all ? _refine_special_details ; ? ; _refine_ls_matrix_type ? _refine_ls_weighting_scheme sigma # options are 'sigma'(based on measured su's) # or 'calc' (calculated weights) _refine_ls_weighting_details 1/(sigma*sigma) _refine_ls_extinction_coef ? _refine_ls_number_parameters 54 _refine_ls_number_restraints ? _refine_ls_number_constraints ? # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.974 _refine_ls_restrained_S_all ? _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 2.0 _pd_proc_2theta_range_max 31.2 _pd_proc_2theta_range_inc 0.001 _pd_proc_wavelength 0.413920 _pd_block_diffractogram_id CuF2(44bipy)_100K # The id used for the block containing # the powder pattern profile (section 11). # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection SPEC _computing_cell_refinement TOPAS _computing_data_reduction TOPAS _computing_structure_solution TOPAS _computing_structure_refinement TOPAS _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu Uani 0.00000 0.00000 0.00000 1.000 0.0165(1) . . . . F1 F Uani -0.1339(3) 0.00000 -0.4157(6) 1.000 0.0202(3) . . . . N1 N Uiso 0.00000 0.18194(11) 0.00000 1.000 0.0065 . . . . C1 C Uiso 0.10576(7) 0.36733(11) 0.1554(4) 1.000 0.0065 . . . . C2 C Uiso 0.10576(7) 0.24448(10) 0.1554(4) 1.000 0.0065 . . . . C3 C Uiso 0.00000 0.42875(14) 0.00000 1.000 0.0065 . . . . H1 H Uiso 0.18918(9) 0.41578(11) 0.2779(7) 1.000 0.0065 . . . . H2 H Uiso 0.18918(9) 0.19603(10) 0.2779(7) 1.000 0.0065 . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0179(2) 0.0095(2) 0.0199(2) 0.0000 -0.0073(1) 0.0000 F1 0.0218(5) 0.0161(4) 0.0197(5) 0.0000 -0.0110(4) 0.0000 #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 F1 1.911(3) . . yes Cu1 N1 2.0279(12) . . yes Cu1 F1 1.911(3) . 2_555 yes Cu1 N1 2.0279(12) . 3_555 yes N1 C2 1.3755(12) . . yes N1 C2 1.3755(12) . 2_555 yes C1 C2 1.3693(17) . . no C1 C3 1.3693(13) . . no C3 C3 1.588(2) . 3_565 no C1 H1 1.0800(17) . . no C2 H2 1.0800(17) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Cu1 N1 90.00(1) . . . yes F1 Cu1 F1 180.00 . . 2_555 yes F1 Cu1 N1 90.00(1) . . 3_555 yes F1 Cu1 N1 90.00(1) 2_555 . . yes N1 Cu1 N1 180.00 . . 3_555 yes F1 Cu1 N1 90.00(1) 2_555 . 3_555 yes Cu1 N1 C2 120.45(6) . . . yes Cu1 N1 C2 120.45(6) . . 2_555 yes C2 N1 C2 119.11(11) . . 2_555 yes C2 C1 C3 120.00(10) . . . no N1 C2 C1 120.45(9) . . . yes C1 C3 C1 120.01(13) . . 2_555 no C1 C3 C3 120.00(7) . . 3_565 no C1 C3 C3 120.00(7) 2_555 . 3_565 no C2 C1 H1 120.00(12) . . . no C3 C1 H1 120.00(13) . . . no N1 C2 H2 119.55(12) . . . no C1 C2 H2 120.00(11) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F1 Cu1 N1 C2 -157.90(10) . . . . no Cu1 N1 C2 C1 180.00(9) . . . . no C2 N1 C2 C1 0.00(15) 2_555 . . . no C2 C1 C3 C3 -180.00(9) . . . 3_565 no C3 C1 C2 N1 0.00(18) . . . . no C2 C1 C3 C1 0.00(15) . . . 2_555 no data_CuF2(44bipy)_RT _database_code_depnum_ccdc_archive 'CCDC 925067' #TrackingRef 'web_deposit_cif_file_4_SaulH.Lapidus_1361228198.CuF2(44bipy)_RT_pub.cif' # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C10 H8 Cu F2 N2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C10 H8 Cu F2 N2' _chemical_formula_weight 257.73 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_length_neutron # include if applicable ? ? ? ? ? ? #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 2/m' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,-z 3 -x,-y,-z 4 x,-y,z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,z _cell_length_a 10.650126(85) _cell_length_b 11.147580(37) _cell_length_c 3.566382(11) _cell_angle_alpha 90 _cell_angle_beta 97.49034(41) _cell_angle_gamma 90 _cell_volume 419.7990(52) _cell_formula_units_Z 2 _cell_measurement_temperature 295 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; capillary ; _pd_spec_mount_mode transmission # options are 'reflection' # or 'transmission' _pd_spec_shape cylinder # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? # include if applicable _exptl_absorpt_correction_type ? # include if applicable _exptl_absorpt_process_details ? # include if applicable _exptl_absorpt_correction_T_min ? # include if applicable _exptl_absorpt_correction_T_max ? # include if applicable #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; 11-BM, APS, Argonne National Lab ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ? ; _diffrn_ambient_temperature 295 _diffrn_source synchrotron _diffrn_source_target ? _diffrn_source_type ? _diffrn_radiation_type synchrotron _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. _diffrn_radiation_wavelength 0.413920 _diffrn_radiation_monochromator 'Si(111) channel cut' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 29201 _pd_meas_2theta_range_min 2.0 _pd_meas_2theta_range_max 31.2 _pd_meas_2theta_range_inc 0.001 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; Molecules are defined as rigid bodies using the z-matrix function implemented in TOPAS. ; # The next three items are given as text. _pd_proc_ls_profile_function ; Simple_Axial_model function with Rp=9999,Rs=1000 in TOPAS ; _pd_proc_ls_background_function ; 2 Pearson-Voight peaks and Chebyshev polynomial with 55 coefficients ; _pd_proc_ls_pref_orient_corr ; none ; _pd_proc_ls_prof_R_factor 0.06968 # 6.968(%) _pd_proc_ls_prof_wR_factor 0.08985 # 8.985(%) _pd_proc_ls_prof_wR_expected 0.05406 # 5.406(%) _refine_ls_R_I_factor ? _refine_ls_R_Fsqd_factor ? _refine_ls_R_factor_all ? _refine_special_details ; ? ; _refine_ls_matrix_type ? _refine_ls_weighting_scheme sigma # options are 'sigma'(based on measured su's) # or 'calc' (calculated weights) _refine_ls_weighting_details 1/(sigma*sigma) _refine_ls_extinction_coef ? _refine_ls_number_parameters 55 _refine_ls_number_restraints ? _refine_ls_number_constraints ? # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.662 _refine_ls_restrained_S_all ? _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 2.0 _pd_proc_2theta_range_max 31.2 _pd_proc_2theta_range_inc 0.001 _pd_proc_wavelength 0.413920 _pd_block_diffractogram_id CuF2(44bipy)_RT # The id used for the block containing # the powder pattern profile (section 11). # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection SPEC _computing_cell_refinement TOPAS _computing_data_reduction TOPAS _computing_structure_solution TOPAS _computing_structure_refinement TOPAS _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu Uani 0.00000 0.00000 0.00000 1.000 0.0166(1) . . . . F1 F Uani -0.13654(18) 0.00000 -0.3993(3) 1.000 0.0204(3) . . . . N1 N Uiso 0.00000 0.18184(8) 0.00000 1.000 0.0152 . . . . C1 C Uiso 0.10526(12) 0.36778(6) 0.1545(3) 1.000 0.0152 . . . . C2 C Uiso 0.10526(12) 0.24524(14) 0.1545(3) 1.000 0.0152 . . . . C3 C Uiso 0.00000 0.42904(10) 0.00000 1.000 0.0152 . . . . H1 H Uiso 0.18848(12) 0.41622(6) 0.2767(5) 1.000 0.0228 . . . . H2 H Uiso 0.18848(12) 0.19680(14) 0.2767(5) 1.000 0.0228 . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0179(2) 0.0095(2) 0.0199(2) 0.0000 -0.0073(1) 0.0000 F1 0.0218(5) 0.0161(4) 0.0197(5) 0.0000 -0.0110(4) 0.0000 #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 F1 1.8981(15) . . yes Cu1 N1 2.0271(9) . . yes Cu1 F1 1.8981(15) . 2_555 yes Cu1 N1 2.0271(9) . 3_555 yes N1 C2 1.3780(14) . . yes N1 C2 1.3780(14) . 2_555 yes C1 C2 1.3660(17) . . no C1 C3 1.3659(13) . . no C3 C3 1.5821(16) . 3_565 no C1 H1 1.0800(17) . . no C2 H2 1.080(2) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Cu1 N1 90.00(1) . . . yes F1 Cu1 F1 180.00 . . 2_555 yes F1 Cu1 N1 90.00(1) . . 3_555 yes F1 Cu1 N1 90.00(1) 2_555 . . yes N1 Cu1 N1 180.00 . . 3_555 yes F1 Cu1 N1 90.00(1) 2_555 . 3_555 yes Cu1 N1 C2 120.86(7) . . . yes Cu1 N1 C2 120.86(7) . . 2_555 yes C2 N1 C2 118.29(11) . . 2_555 yes C2 C1 C3 120.00(11) . . . no N1 C2 C1 120.86(11) . . . yes C1 C3 C1 120.00(10) . . 2_555 no C1 C3 C3 120.00(5) . . 3_565 no C1 C3 C3 120.00(5) 2_555 . 3_565 no C2 C1 H1 120.00(11) . . . no C3 C1 H1 120.00(8) . . . no N1 C2 H2 119.14(15) . . . no C1 C2 H2 120.00(15) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F1 Cu1 N1 C2 -159.44(7) . . . . no Cu1 N1 C2 C1 180.00(7) . . . . no C2 N1 C2 C1 0.00(13) 2_555 . . . no C2 C1 C3 C3 -179.98(9) . . . 3_565 no C3 C1 C2 N1 0.00(15) . . . . no C2 C1 C3 C1 0.00(13) . . . 2_555 no data_CuF2pyz_100K _database_code_depnum_ccdc_archive 'CCDC 925068' #TrackingRef 'web_deposit_cif_file_5_SaulH.Lapidus_1361228198.CuF2pyz_100K_pub.cif' # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C4 H4 Cu F2 N2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H4 Cu F2 N2' _chemical_formula_weight 181.64 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_length_neutron # include if applicable ? ? ? ? ? ? #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 2/m' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,-z 3 -x,-y,-z 4 x,-y,z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,z _cell_length_a 10.236569(68) _cell_length_b 6.863715(21) _cell_length_c 3.351077(27) _cell_angle_alpha 90 _cell_angle_beta 92.70769(39) _cell_angle_gamma 90 _cell_volume 235.1868(34) _cell_formula_units_Z ? _cell_measurement_temperature 100 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; ? ; _pd_spec_mount_mode transmission # options are 'reflection' # or 'transmission' _pd_spec_shape cylinder # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? # include if applicable _exptl_absorpt_correction_type ? # include if applicable _exptl_absorpt_process_details ? # include if applicable _exptl_absorpt_correction_T_min ? # include if applicable _exptl_absorpt_correction_T_max ? # include if applicable #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; 11-BM, Advanced Photon Source, Argonne National Laboratory ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; LaB6 ; _diffrn_ambient_temperature 100 _diffrn_source synchrotron _diffrn_source_target ? _diffrn_source_type ? _diffrn_radiation_type synchrotron _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. _diffrn_radiation_wavelength 0.413920 _diffrn_radiation_monochromator 'Si(111) channel cut' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 32001 _pd_meas_2theta_range_min 2.0 _pd_meas_2theta_range_max 34.0 _pd_meas_2theta_range_inc 0.001 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; Molecules are defined as rigid bodies using the z-matrix function implemented in TOPAS. ; # The next three items are given as text. _pd_proc_ls_profile_function ; Simple_Axial_model function with Rp=9999,Rs=1000 in TOPAS-Academic ; _pd_proc_ls_background_function ; 0 Pearson-Voight peaks and Chebyshev polynomial with 10 coefficients ; _pd_proc_ls_pref_orient_corr ; none ; _pd_proc_ls_prof_R_factor 0.08757 # 8.757(%) _pd_proc_ls_prof_wR_factor 0.11757 # 11.757(%) _pd_proc_ls_prof_wR_expected 0.04939 # 4.939(%) _refine_ls_R_I_factor ? _refine_ls_R_Fsqd_factor ? _refine_ls_R_factor_all ? _refine_special_details ; ? ; _refine_ls_matrix_type ? _refine_ls_weighting_scheme sigma # options are 'sigma'(based on measured su's) # or 'calc' (calculated weights) _refine_ls_weighting_details 1/(sigma*sigma) _refine_ls_extinction_coef ? _refine_ls_number_parameters 66 _refine_ls_number_restraints ? _refine_ls_number_constraints ? # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 2.380 _refine_ls_restrained_S_all ? _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 2.0 _pd_proc_2theta_range_max 34.0 _pd_proc_2theta_range_inc 0.001 _pd_proc_wavelength 0.413920 _pd_block_diffractogram_id CuF2pyz_100K # The id used for the block containing # the powder pattern profile (section 11). # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection SPEC _computing_cell_refinement TOPAS _computing_data_reduction TOPAS _computing_structure_solution TOPAS _computing_structure_refinement TOPAS _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu Uiso 0.00000 0.50000 1.00000 1.000 0.0161(1) . . . . F1 F Uiso -0.13392(10) 0.50000 0.5881(3) 1.000 0.0197(3) . . . . N1 N Uiso 0.00000 0.2035(3) 1.00000 1.000 0.0110(4) . . . . C1 C Uiso 0.10453(7) 0.1012(3) 1.1370(5) 1.000 0.0106(3) . . . . H1 H Uiso 0.19199 0.1768 1.2517 1.000 0.026(3) . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0179(2) 0.0095(2) 0.0199(2) 0.0000 -0.0073(1) 0.0000 F1 0.0218(5) 0.0161(4) 0.0197(5) 0.0000 -0.0110(4) 0.0000 N1 0.0159(7) 0.0097(6) 0.0073(7) 0.0000 0.0008(5) 0.0000 C1 0.0106(6) 0.0146(5) 0.0067(6) 0.0005(4) 0.0017(4) -0.0004(4) # Note: if the displacement parameters were refined anisotropically # the U matrices should be given as for single-crystal studies. # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 F1 1.8989(10) . . yes Cu1 N1 2.035(2) . . yes Cu1 F1 2.4533(10) . 1_556 yes Cu1 F1 2.4533(10) . 2_556 yes Cu1 F1 1.8989(10) . 2_557 yes Cu1 N1 2.035(2) . 3_567 yes N1 C1 1.3425(17) . . yes N1 C1 1.3425(17) . 2_557 yes C1 C1 1.389(3) . 4_555 no C1 H1 1.089 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Cu1 N1 90.00(1) . . . yes F1 Cu1 F1 99.92(4) . . 1_556 yes F1 Cu1 F1 80.08(4) . . 2_556 yes F1 Cu1 F1 180.00 . . 2_557 yes F1 Cu1 N1 90.00(1) . . 3_567 yes F1 Cu1 N1 90.00(1) 1_556 . . yes F1 Cu1 N1 90.00(1) 2_556 . . yes F1 Cu1 N1 90.00(1) 2_557 . . yes N1 Cu1 N1 180.00 . . 3_567 yes F1 Cu1 F1 180.00 1_556 . 2_556 yes F1 Cu1 F1 80.08(4) 1_556 . 2_557 yes F1 Cu1 N1 90.00(1) 1_556 . 3_567 yes F1 Cu1 F1 99.92(4) 2_556 . 2_557 yes F1 Cu1 N1 90.00(1) 2_556 . 3_567 yes F1 Cu1 N1 90.00(1) 2_557 . 3_567 yes Cu1 F1 Cu1 99.92(4) . . 1_554 yes Cu1 N1 C1 121.54(11) . . . yes Cu1 N1 C1 121.54(11) . . 2_557 yes C1 N1 C1 116.93(19) . . 2_557 yes N1 C1 C1 121.54(13) . . 4_555 yes N1 C1 H1 120.0 . . . no C1 C1 H1 118.46 4_555 . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F1 Cu1 N1 C1 157.07(8) . . . . no Cu1 N1 C1 C1 -180.00(11) . . . 4_555 no data_CuF2pyz_RT _database_code_depnum_ccdc_archive 'CCDC 925069' #TrackingRef 'web_deposit_cif_file_6_SaulH.Lapidus_1361228198.CuF2pyz_RT_pub.cif' # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C4 H4 Cu F2 N2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H4 Cu F2 N2' _chemical_formula_weight 181.64 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_length_neutron # include if applicable ? ? ? ? ? ? #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2y' _symmetry_space_group_name_H-M 'C 2/m' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,-z 3 -x,-y,-z 4 x,-y,z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,z _cell_length_a 10.311472(16) _cell_length_b 6.872494(8) _cell_length_c 3.380942(5) _cell_angle_alpha 90 _cell_angle_beta 93.38898(10) _cell_angle_gamma 90 _cell_volume 239.17325(60) _cell_formula_units_Z 2 _cell_measurement_temperature 295 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; capillary ; _pd_spec_mount_mode transmission # options are 'reflection' # or 'transmission' _pd_spec_shape cylinder # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? # include if applicable _exptl_absorpt_correction_type ? # include if applicable _exptl_absorpt_process_details ? # include if applicable _exptl_absorpt_correction_T_min ? # include if applicable _exptl_absorpt_correction_T_max ? # include if applicable #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; 11-BM, Advanced Photon Source, Argonne National Laboratory ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; NIST standard reference material 1976(sintered plate of Al2O3) Well-isolated 7 reflections were used to calibrate wavelength and detector zero. ; _diffrn_ambient_temperature 295 _diffrn_source synchrotron _diffrn_source_target ? _diffrn_source_type ? _diffrn_radiation_type synchrotron _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method step # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. _diffrn_radiation_wavelength 0.413920 _diffrn_radiation_monochromator 'Si(111) channel cut' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 29201 _pd_meas_2theta_range_min 2.0 _pd_meas_2theta_range_max 31.2 _pd_meas_2theta_range_inc 0.001 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; Molecules are defined as rigid bodies using the z-matrix function implemented in TOPAS. ; # The next three items are given as text. _pd_proc_ls_profile_function ; Simple_Axial_model function with Rp=9999,Rs=1000 in TOPAS ; _pd_proc_ls_background_function ; 1 Pearson-Voight peaks and Chebyshev polynomial with 10 coefficients ; _pd_proc_ls_pref_orient_corr ; none ; _pd_proc_ls_prof_R_factor 0.05445 # 5.445(%) _pd_proc_ls_prof_wR_factor 0.07656 # 7.656(%) _pd_proc_ls_prof_wR_expected 0.0481 # 4.810(%) _refine_ls_R_I_factor ? _refine_ls_R_Fsqd_factor ? _refine_ls_R_factor_all ? _refine_special_details ; ? ; _refine_ls_matrix_type ? _refine_ls_weighting_scheme sigma # options are 'sigma'(based on measured su's) # or 'calc' (calculated weights) _refine_ls_weighting_details 1/(sigma*sigma) _refine_ls_extinction_coef ? _refine_ls_number_parameters 64 _refine_ls_number_restraints ? _refine_ls_number_constraints ? # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 1.592 _refine_ls_restrained_S_all ? _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 2.0 _pd_proc_2theta_range_max 31.2 _pd_proc_2theta_range_inc 0.001 _pd_proc_wavelength 0.413920 _pd_block_diffractogram_id CuF2pyz_RT # The id used for the block containing # the powder pattern profile (section 11). # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_cell_refinement TOPAS _computing_data_reduction TOPAS _computing_structure_solution TOPAS _computing_structure_refinement TOPAS _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu Uani 0.00000 0.50000 1.00000 1.000 0.0161(1) . . . . F1 F Uani -0.13344(6) 0.50000 0.5926(2) 1.000 0.0197(3) . . . . N1 N Uani 0.00000 0.20229 1.00000 1.000 0.0110(4) . . . . C1 C Uani 0.10391 0.10074 1.13580 1.000 0.0106(3) . . . . H1 H Uiso 0.19107 0.17644 1.24971 1.000 0.026(3) . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0179(2) 0.0095(2) 0.0199(2) 0.0000 -0.0073(1) 0.0000 F1 0.0218(5) 0.0161(4) 0.0197(5) 0.0000 -0.0110(4) 0.0000 N1 0.0159(7) 0.0097(6) 0.0073(7) 0.0000 0.0008(5) 0.0000 C1 0.0106(6) 0.0146(5) 0.0067(6) 0.0005(4) 0.0017(4) -0.0004(4) #=============================================================================== # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 F1 1.8885(6) . . yes Cu1 N1 2.0460(1) . . yes Cu1 F1 2.4967(7) . 1_556 yes Cu1 F1 2.4967(7) . 2_556 yes Cu1 F1 1.8885(7) . 2_557 yes Cu1 N1 2.0460(1) . 3_567 yes N1 C1 1.3370 . . yes N1 C1 1.3370 . 2_557 yes C1 C1 1.3847 . 4_555 no C1 H1 1.0900 . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Cu1 N1 90.00(1) . . . yes F1 Cu1 F1 99.96(2) . . 1_556 yes F1 Cu1 F1 80.04(2) . . 2_556 yes F1 Cu1 F1 180.00 . . 2_557 yes F1 Cu1 N1 90.00(1) . . 3_567 yes F1 Cu1 N1 90.00(1) 1_556 . . yes F1 Cu1 N1 90.00(1) 2_556 . . yes F1 Cu1 N1 90.00(1) 2_557 . . yes N1 Cu1 N1 180.00 . . 3_567 yes F1 Cu1 F1 180.00 1_556 . 2_556 yes F1 Cu1 F1 80.04(2) 1_556 . 2_557 yes F1 Cu1 N1 90.00(1) 1_556 . 3_567 yes F1 Cu1 F1 99.96(2) 2_556 . 2_557 yes F1 Cu1 N1 90.00(1) 2_556 . 3_567 yes F1 Cu1 N1 90.00(1) 2_557 . 3_567 yes Cu1 F1 Cu1 99.96(3) . . 1_554 yes Cu1 N1 C1 121.46 . . . yes Cu1 N1 C1 121.46 . . 2_557 yes C1 N1 C1 117.07 . . 2_557 yes N1 C1 C1 121.46 . . 4_555 yes N1 C1 H1 120.00 . . . no C1 C1 H1 119.00 4_555 . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F1 Cu1 N1 C1 156.97 . . . . no Cu1 N1 C1 C1 -180.00 . . . 4_555 no data_JAS1661C_12K _database_code_depnum_ccdc_archive 'CCDC 925070' #TrackingRef 'web_deposit_cif_file_7_SaulH.Lapidus_1361228198.JAS1661C_12K_pub.cif' # 5. CHEMICAL DATA _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C4 H4 Cu F2 N2' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C4 H4 Cu F2 N2' _chemical_formula_weight 181.64 _chemical_melting_point ? _chemical_compound_source ? # for minerals and # natural products loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source _atom_type_scat_length_neutron # include if applicable ? ? ? ? ? ? #============================================================================== # 6. POWDER SPECIMEN AND CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/m _symmetry_space_group_name_Hall '-C 2y' _symmetry_Int_Tables_number 12 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 x,y,z 2 -x,y,-z 3 -x,-y,-z 4 x,-y,z 5 1/2+x,1/2+y,z 6 1/2-x,1/2+y,-z 7 1/2-x,1/2-y,-z 8 1/2+x,1/2-y,z _cell_length_a 10.23459(18) _cell_length_b 6.86586(22) _cell_length_c 3.34733(12) _cell_angle_alpha 90 _cell_angle_beta 92.6265(26) _cell_angle_gamma 90 _cell_volume 234.9673(96) _cell_formula_units_Z 2 _cell_measurement_temperature 295 _cell_special_details ; ? ; # The next three fields give the specimen dimensions in mm. The equatorial # plane contains the incident and diffracted beam. _pd_spec_size_axial ? # perpendicular to # equatorial plane _pd_spec_size_equat ? # parallel to # scattering vector # in transmission _pd_spec_size_thick ? # parallel to # scattering vector # in reflection # The next five fields are character fields that describe the specimen. _pd_spec_mounting # This field should be # used to give details of the # container. ; capillary ; _pd_spec_mount_mode reflection # options are 'reflection' # or 'transmission' _pd_spec_shape flat_sheet # options are 'cylinder' # 'flat_sheet' or 'irregular' _pd_char_particle_morphology ? _pd_char_colour ? # use ICDD colour descriptions # The following three fields describe the preparation of the specimen. # The cooling rate is in K/min. The pressure at which the sample was # prepared is in kPa. The temperature of preparation is in K. _pd_prep_cool_rate ? _pd_prep_pressure ? _pd_prep_temperature ? # The next four fields are normally only needed for transmission experiments. _exptl_absorpt_coefficient_mu ? # include if applicable _exptl_absorpt_correction_type ? # include if applicable _exptl_absorpt_process_details ? # include if applicable _exptl_absorpt_correction_T_min ? # include if applicable _exptl_absorpt_correction_T_max ? # include if applicable #============================================================================== # 7. EXPERIMENTAL DATA _exptl_special_details ; ? ; # The following item is used to identify the equipment used to record # the powder pattern when the diffractogram was measured at a laboratory # other than the authors' home institution, e.g. when neutron or synchrotron # radiation is used. _pd_instr_location ; Argonne National Lab ; _pd_calibration_special_details # description of the method used # to calibrate the instrument ; ; _diffrn_ambient_temperature 295 _diffrn_source CuKalpha _diffrn_source_target ? _diffrn_source_type ? _diffrn_radiation_type ? _diffrn_measurement_device_type ? _diffrn_detector ? _diffrn_detector_type ? # make or model of detector _pd_meas_scan_method cont # options are 'step', 'cont', # 'tof', 'fixed' or # 'disp' (= dispersive) _pd_meas_special_details ; ? ; # The following six items are used for angular dispersive measurements only. _diffrn_radiation_wavelength 1.534753 _diffrn_radiation_monochromator 'Si(111) channel cut' # The following four items give details of the measured (not processed) # powder pattern. Angles are in degrees. _pd_meas_number_of_points 3294 _pd_meas_2theta_range_min 14.008 _pd_meas_2theta_range_max 69.989 _pd_meas_2theta_range_inc 0.017 # The following three items are used for time-of-flight measurements only. _pd_instr_dist_src/spec ? _pd_instr_dist_spec/detc ? _pd_meas_2theta_fixed ? #============================================================================== # 8. REFINEMENT DATA # Use the next field to give any special details about the fitting of the # powder pattern. _pd_proc_ls_special_details ; Molecules are defined as rigid bodies using the z-matrix function implemented in TOPAS. ; # The next three items are given as text. _pd_proc_ls_profile_function ; Simple_Axial_model function with Rp=240,Rs=240 in TOPAS ; _pd_proc_ls_background_function ; 1 Pearson-Voight peaks and Chebyshev polynomial with 8 coefficients ; _pd_proc_ls_pref_orient_corr ; none ; _pd_proc_ls_prof_R_factor 0.03702 # 3.702(%) _pd_proc_ls_prof_wR_factor 0.05184 # 5.184(%) _pd_proc_ls_prof_wR_expected 0.01725 # 1.725(%) _refine_ls_R_I_factor ? _refine_ls_R_Fsqd_factor ? _refine_ls_R_factor_all ? _refine_special_details ; ? ; _refine_ls_matrix_type ? _refine_ls_weighting_scheme sigma # options are 'sigma'(based on measured su's) # or 'calc' (calculated weights) _refine_ls_weighting_details 1/(sigma*sigma) _refine_ls_extinction_coef ? _refine_ls_number_parameters 34 _refine_ls_number_restraints ? _refine_ls_number_constraints ? # The following item is the same as CHI, the square root of 'CHI squared' _refine_ls_goodness_of_fit_all 3.005 _refine_ls_restrained_S_all ? _refine_ls_shift/su_max ? _refine_ls_shift/su_mean ? # The following four items apply to angular dispersive measurements. # 2theta minimum, maximum and increment (in degrees) are for the # intensities used in the refinement. _pd_proc_2theta_range_min 14.008 _pd_proc_2theta_range_max 69.989 _pd_proc_2theta_range_inc 0.017 _pd_proc_wavelength 1.534753 _pd_block_diffractogram_id JAS1661C_12K # The id used for the block containing # the powder pattern profile (section 11). # Give appropriate details in the next two text fields. _pd_proc_info_excluded_regions ? _pd_proc_info_data_reduction ? # The following items are used to identify the programs used. _computing_data_collection ? _computing_cell_refinement TOPAS _computing_data_reduction TOPAS _computing_structure_solution TOPAS _computing_structure_refinement TOPAS _computing_molecular_graphics ? _computing_publication_material ? #============================================================================== # 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu Uiso 0.00000 0.50000 1.00000 1.000 0.0255(16) . . . . F1 F Uiso -0.1347(3) 0.50000 0.5801(18) 1.000 0.0109 . . . . N1 N Uiso 0.00000 0.196(2) 1.00000 1.000 0.0109 . . . . C1 C Uiso 0.1059(6) 0.0994(8) 1.1363(11) 1.000 0.0109 . . . . H1 H Uiso 0.1922(3) 0.179(2) 1.247(2) 1.000 0.0109 . . . . # 10. MOLECULAR GEOMETRY _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 F1 1.923(5) . . yes Cu1 N1 2.087(14) . . yes Cu1 F1 2.432(5) . 1_556 yes Cu1 F1 2.432(5) . 2_556 yes Cu1 F1 1.923(5) . 2_557 yes Cu1 N1 2.087(14) . 3_567 yes N1 C1 1.333(9) . . yes N1 C1 1.333(9) . 2_557 yes C1 C1 1.365(8) . 4_555 no C1 H1 1.089(10) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag F1 Cu1 N1 90.00(1) . . . yes F1 Cu1 F1 99.78(17) . . 1_556 yes F1 Cu1 F1 80.22(17) . . 2_556 yes F1 Cu1 F1 180.00 . . 2_557 yes F1 Cu1 N1 90.00(1) . . 3_567 yes F1 Cu1 N1 90.00(1) 1_556 . . yes F1 Cu1 N1 90.00(1) 2_556 . . yes F1 Cu1 N1 90.00(1) 2_557 . . yes N1 Cu1 N1 180.00 . . 3_567 yes F1 Cu1 F1 180.00 1_556 . 2_556 yes F1 Cu1 F1 80.22(17) 1_556 . 2_557 yes F1 Cu1 N1 90.00(1) 1_556 . 3_567 yes F1 Cu1 F1 99.78(17) 2_556 . 2_557 yes F1 Cu1 N1 90.00(1) 2_556 . 3_567 yes F1 Cu1 N1 90.00(1) 2_557 . 3_567 yes Cu1 F1 Cu1 99.78(13) . . 1_554 yes Cu1 N1 C1 119.8(6) . . . yes Cu1 N1 C1 119.8(6) . . 2_557 yes C1 N1 C1 120.3(11) . . 2_557 yes N1 C1 C1 119.8(7) . . 4_555 yes N1 C1 H1 120.1(9) . . . no C1 C1 H1 120.1(8) 4_555 . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F1 Cu1 N1 C1 156.3(2) . . . . no Cu1 N1 C1 C1 -180.0(3) . . . 4_555 no