Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemsitry 2002 data_ak1 _database_code_CSD 168372 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Knight, D Andrew' 'Butcher, Raymond J.' 'Harper, Brandy A.' 'Kim, Vinny' 'Schull, Terence L.' _publ_contact_author_name 'Dr D Andrew Knight' _publ_contact_author_address ; Department of Chemistry Loyola University 6363 St Charles Avenue, New Orleans Louisiana 70118 UNITED STATES OF AMERICA ; _publ_contact_author_email 'DAKNIGHT@LOYNO.EDU' _publ_section_title ; Rhodium-mediated Delamination of Layered Copper and Zinc Vinylphosphonates ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H5 Cu O4 P' _chemical_formula_weight 187.57 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.878(5) _cell_length_b 7.628(3) _cell_length_c 7.332(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.97(3) _cell_angle_gamma 90.00 _cell_volume 549.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 36 _cell_measurement_theta_min 5.44 _cell_measurement_theta_max 12.47 _exptl_crystal_description CHUNK _exptl_crystal_colour BLUE _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 372 _exptl_absorpt_coefficient_mu 4.183 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.3778 _exptl_absorpt_correction_T_max 0.4859 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 1354 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 27.48 _reflns_number_total 1254 _reflns_number_gt 1155 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.0845P)^2^+0.5496P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.011(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1254 _refine_ls_number_parameters 83 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1216 _refine_ls_wR_factor_gt 0.1187 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.001 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 Cu Cu 0.54326(4) 0.31018(5) 0.06504(5) 0.0153(2) Uani 1 1 d . . . P P 0.34179(8) 0.05008(11) -0.17736(11) 0.0128(3) Uani 1 1 d . . . O1W O 0.7050(3) 0.4332(4) 0.1931(4) 0.0209(6) Uani 1 1 d D . . H1W1 H 0.676(7) 0.525(7) 0.161(7) 0.06(2) Uiso 1 1 d D . . H1W2 H 0.695(8) 0.435(8) 0.298(6) 0.07(2) Uiso 1 1 d D . . O1 O 0.3807(3) 0.2252(3) -0.0853(4) 0.0196(5) Uani 1 1 d . . . O2 O 0.3492(3) -0.1017(3) -0.0397(3) 0.0174(5) Uani 1 1 d . . . O3 O 0.4288(3) 0.0084(3) -0.3344(3) 0.0168(5) Uani 1 1 d . . . C1 C 0.1696(4) 0.0738(6) -0.2717(6) 0.0281(8) Uani 1 1 d . . . H1A H 0.1485 0.1644 -0.3546 0.034 Uiso 1 1 calc R . . C2 C 0.0708(5) -0.0288(9) -0.2312(9) 0.0591(16) Uani 1 1 d . . . H2A H 0.0889 -0.1205 -0.1486 0.071 Uiso 1 1 calc R . . H2B H -0.0175 -0.0100 -0.2849 0.071 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 Cu 0.0198(3) 0.0113(3) 0.0146(3) -0.00175(13) 0.00064(19) 0.00079(14) P 0.0153(4) 0.0103(4) 0.0126(4) -0.0001(3) 0.0008(3) 0.0003(3) O1W 0.0232(13) 0.0215(14) 0.0178(12) -0.0013(10) 0.0012(10) -0.0003(11) O1 0.0240(12) 0.0105(11) 0.0233(13) -0.0038(9) -0.0030(10) 0.0003(10) O2 0.0261(13) 0.0126(11) 0.0142(11) 0.0035(9) 0.0053(9) 0.0032(9) O3 0.0241(12) 0.0147(12) 0.0120(11) -0.0002(8) 0.0039(9) -0.0002(9) C1 0.0212(18) 0.031(2) 0.030(2) -0.0002(17) -0.0042(15) 0.0032(15) C2 0.025(2) 0.072(4) 0.079(4) 0.009(3) -0.005(2) -0.012(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 Cu O2 1.932(3) 3_655 ? Cu O1 1.961(3) . ? Cu O3 1.978(3) 4_566 ? Cu O1W 2.001(3) . ? Cu O3 2.306(2) 2_654 ? P O1 1.527(3) . ? P O2 1.533(2) . ? P O3 1.540(2) . ? P C1 1.777(4) . ? O2 Cu 1.932(3) 3_655 ? O3 Cu 1.978(3) 4_565 ? O3 Cu 2.306(2) 2_644 ? C1 C2 1.309(7) . ? 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 O2 Cu O1 95.72(11) 3_655 . ? O2 Cu O3 162.41(10) 3_655 4_566 ? O1 Cu O3 88.54(11) . 4_566 ? O2 Cu O1W 90.65(12) 3_655 . ? O1 Cu O1W 170.43(11) . . ? O3 Cu O1W 87.50(11) 4_566 . ? O2 Cu O3 111.11(9) 3_655 2_654 ? O1 Cu O3 87.60(10) . 2_654 ? O3 Cu O3 86.07(10) 4_566 2_654 ? O1W Cu O3 83.44(11) . 2_654 ? O1 P O2 112.13(14) . . ? O1 P O3 112.11(15) . . ? O2 P O3 110.13(14) . . ? O1 P C1 105.65(18) . . ? O2 P C1 108.15(18) . . ? O3 P C1 108.42(17) . . ? P O1 Cu 133.74(16) . . ? P O2 Cu 123.20(14) . 3_655 ? P O3 Cu 121.30(15) . 4_565 ? P O3 Cu 143.36(15) . 2_644 ? Cu O3 Cu 93.93(10) 4_565 2_644 ? C2 C1 P 123.8(4) . . ? 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 O2 P O1 Cu 57.3(3) . . . . ? O3 P O1 Cu -67.2(3) . . . . ? C1 P O1 Cu 174.9(2) . . . . ? O2 Cu O1 P 5.5(2) 3_655 . . . ? O3 Cu O1 P -157.4(2) 4_566 . . . ? O1W Cu O1 P 137.1(6) . . . . ? O3 Cu O1 P 116.5(2) 2_654 . . . ? O1 P O2 Cu -124.62(18) . . . 3_655 ? O3 P O2 Cu 1.0(2) . . . 3_655 ? C1 P O2 Cu 119.3(2) . . . 3_655 ? O1 P O3 Cu -13.4(2) . . . 4_565 ? O2 P O3 Cu -138.96(16) . . . 4_565 ? C1 P O3 Cu 102.9(2) . . . 4_565 ? O1 P O3 Cu -175.5(2) . . . 2_644 ? O2 P O3 Cu 58.9(3) . . . 2_644 ? C1 P O3 Cu -59.3(3) . . . 2_644 ? O1 P C1 C2 -122.7(5) . . . . ? O2 P C1 C2 -2.4(5) . . . . ? O3 P C1 C2 117.0(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1W1 O1 0.79(4) 2.04(4) 2.827(4) 174(7) 3_665 O1W H1W1 O3 0.79(4) 2.51(5) 2.875(4) 110(5) 2_654 O1W H1W2 O2 0.79(4) 1.89(4) 2.664(4) 169(7) 2_655 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 4.334 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.184