data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Mercedes Cano' _publ_contact_author_email MMCANO@QUIM.UCM.ES _publ_section_title ; Silver and gold luminescent metallomesogens based on pyrazole ligands ; loop_ _publ_author_name 'Mercedes Cano' 'Jose Antonio Campo' 'J V Heras' 'Carlos Lodeiro' 'Maria Jose Mayoral' 'P Ovejero' ; E.Pinilla ; 'Maria Rosario Torres' data_[C26H32N4Ag][PO2F2] _database_code_depnum_ccdc_archive 'CCDC 688083' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H32 Ag F2 N4 O4 P' _chemical_formula_weight 641.40 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' 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.047(4) _cell_length_b 7.9262(13) _cell_length_c 16.167(3) _cell_angle_alpha 90.00 _cell_angle_beta 117.768(3) _cell_angle_gamma 90.00 _cell_volume 2840.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.500 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.817 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10553 _diffrn_reflns_av_R_equivalents 0.1584 _diffrn_reflns_av_sigmaI/netI 0.1723 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2511 _reflns_number_gt 1001 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker 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^)+(0.0949P)^2^+0.0000P] 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 2511 _refine_ls_number_parameters 160 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1771 _refine_ls_R_factor_gt 0.0652 _refine_ls_wR_factor_ref 0.2017 _refine_ls_wR_factor_gt 0.1571 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.013 _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 Ag Ag 0.0000 0.28882(15) 0.7500 0.0680(5) Uani 1 2 d S . . P P 0.0000 0.7804(5) 0.7500 0.0618(10) Uani 1 2 d S . . O2 O 0.0364(3) 0.6919(10) 0.7184(6) 0.108(3) Uani 1 1 d . . . N1 N 0.0345(3) 0.2837(10) 0.6547(5) 0.0551(19) Uani 1 1 d . . . O1 O 0.1723(3) 0.9004(10) 0.4369(6) 0.101(3) Uani 1 1 d . . . N2 N 0.0545(3) 0.4244(10) 0.6309(5) 0.054(2) Uani 1 1 d . . . H2 H 0.0521 0.5157 0.6720 0.06(3) Uiso 1 1 d R . . F F 0.0393(3) 0.9058(7) 0.8235(4) 0.0921(19) Uani 1 1 d . . . C3 C 0.0735(3) 0.3930(12) 0.5659(6) 0.047(2) Uani 1 1 d . . . C4 C 0.0654(4) 0.2225(13) 0.5488(7) 0.064(3) Uani 1 1 d . . . H4 H 0.0741 0.1603 0.5078 0.077 Uiso 1 1 calc R . . C5 C 0.0422(4) 0.1637(13) 0.6039(7) 0.064(3) Uani 1 1 d . . . H5 H 0.0325 0.0510 0.6059 0.077 Uiso 1 1 calc R . . C6 C 0.0976(4) 0.5257(13) 0.5309(6) 0.051(2) Uani 1 1 d . . . C7 C 0.1100(4) 0.6893(14) 0.5690(7) 0.067(3) Uani 1 1 d . . . H7 H 0.1005 0.7188 0.6163 0.081 Uiso 1 1 calc R . . C8 C 0.1362(5) 0.8046(14) 0.5361(8) 0.078(3) Uani 1 1 d . . . H8 H 0.1467 0.9099 0.5646 0.094 Uiso 1 1 calc R . . C9 C 0.1472(4) 0.7696(16) 0.4629(8) 0.068(3) Uani 1 1 d . . . C10 C 0.1334(4) 0.6168(17) 0.4230(7) 0.067(3) Uani 1 1 d . . . H10 H 0.1397 0.5936 0.3718 0.080 Uiso 1 1 calc R . . C11 C 0.1098(4) 0.4924(13) 0.4575(7) 0.066(3) Uani 1 1 d . . . H11 H 0.1021 0.3855 0.4307 0.079 Uiso 1 1 calc R . . C12 C 0.1851(6) 0.8704(18) 0.3611(10) 0.124(5) Uani 1 1 d D . . H12A H 0.1479 0.8602 0.3030 0.149 Uiso 1 1 calc R . . H12B H 0.2080 0.7670 0.3712 0.149 Uiso 1 1 calc R . . C13 C 0.2217(8) 1.0207(17) 0.3568(13) 0.191(8) Uiso 1 1 d D . . H13A H 0.2597 1.0207 0.4139 0.229 Uiso 1 1 calc R . . H13B H 0.2309 1.0014 0.3055 0.229 Uiso 1 1 calc R . . C14 C 0.1950(9) 1.195(2) 0.3448(15) 0.212(9) Uiso 1 1 d D . . H14A H 0.1913 1.2268 0.3998 0.254 Uiso 1 1 calc R . . H14B H 0.1553 1.1980 0.2910 0.254 Uiso 1 1 calc R . . C15 C 0.2377(8) 1.314(2) 0.3307(13) 0.173(7) Uiso 1 1 d D . . H15A H 0.2743 1.3247 0.3884 0.260 Uiso 1 1 calc R . . H15B H 0.2190 1.4221 0.3115 0.260 Uiso 1 1 calc R . . H15C H 0.2467 1.2689 0.2834 0.260 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 Ag 0.0869(9) 0.0671(9) 0.0744(9) 0.000 0.0581(7) 0.000 P 0.076(2) 0.051(2) 0.068(3) 0.000 0.042(2) 0.000 O2 0.101(5) 0.110(6) 0.129(7) -0.056(5) 0.067(5) 0.013(5) N1 0.068(5) 0.047(5) 0.060(5) 0.004(5) 0.038(4) 0.000(4) O1 0.100(6) 0.094(6) 0.128(7) 0.026(5) 0.067(6) -0.009(5) N2 0.064(5) 0.056(6) 0.056(5) -0.006(4) 0.040(4) -0.001(4) F 0.110(5) 0.067(4) 0.088(4) -0.041(4) 0.038(4) -0.014(4) C3 0.052(5) 0.051(7) 0.043(6) 0.005(5) 0.024(5) 0.002(5) C4 0.096(7) 0.055(7) 0.061(7) -0.008(6) 0.053(6) 0.003(6) C5 0.094(7) 0.051(7) 0.068(7) -0.010(5) 0.054(6) -0.009(5) C6 0.045(5) 0.064(7) 0.045(6) 0.003(5) 0.022(5) 0.002(5) C7 0.072(6) 0.062(7) 0.084(8) -0.016(7) 0.050(6) -0.009(6) C8 0.091(8) 0.048(7) 0.112(9) -0.003(7) 0.060(7) -0.010(6) C9 0.058(6) 0.079(9) 0.074(8) 0.015(7) 0.037(6) -0.002(6) C10 0.064(6) 0.086(9) 0.056(7) 0.001(7) 0.033(6) -0.004(6) C11 0.069(6) 0.075(8) 0.068(7) -0.010(6) 0.044(6) -0.013(6) C12 0.133(11) 0.136(12) 0.150(13) 0.061(10) 0.105(11) -0.012(9) _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 Ag N1 2.089(7) . ? Ag N1 2.089(7) 2_556 ? P O2 1.420(6) . ? P O2 1.420(6) 2_556 ? P F 1.510(5) . ? P F 1.510(5) 2_556 ? N1 C5 1.328(11) . ? N1 N2 1.350(9) . ? O1 C9 1.376(12) . ? O1 C12 1.424(14) . ? N2 C3 1.362(10) . ? N2 H2 1.0029 . ? C3 C4 1.375(12) . ? C3 C6 1.454(12) . ? C4 C5 1.353(12) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C11 1.381(11) . ? C6 C7 1.407(12) . ? C7 C8 1.368(13) . ? C7 H7 0.9300 . ? C8 C9 1.363(14) . ? C8 H8 0.9300 . ? C9 C10 1.340(14) . ? C10 C11 1.393(13) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.524(5) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.505(5) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 C15 1.519(5) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 Ag N1 177.8(5) . 2_556 ? O2 P O2 120.8(8) . 2_556 ? O2 P F 108.4(4) . . ? O2 P F 109.6(5) 2_556 . ? O2 P F 109.6(4) . 2_556 ? O2 P F 108.4(4) 2_556 2_556 ? F P F 97.6(5) . 2_556 ? C5 N1 N2 103.6(7) . . ? C5 N1 Ag 134.3(7) . . ? N2 N1 Ag 122.0(6) . . ? C9 O1 C12 117.1(10) . . ? C3 N2 N1 112.2(7) . . ? C3 N2 H2 142.4 . . ? N1 N2 H2 105.2 . . ? N2 C3 C4 105.2(7) . . ? N2 C3 C6 121.8(9) . . ? C4 C3 C6 133.0(9) . . ? C5 C4 C3 106.0(8) . . ? C5 C4 H4 127.0 . . ? C3 C4 H4 127.0 . . ? N1 C5 C4 113.0(9) . . ? N1 C5 H5 123.5 . . ? C4 C5 H5 123.5 . . ? C11 C6 C7 117.4(9) . . ? C11 C6 C3 119.7(9) . . ? C7 C6 C3 122.9(8) . . ? C6 C7 C8 119.6(10) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 C7 121.9(11) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C10 C9 C8 119.5(10) . . ? C10 C9 O1 125.8(11) . . ? C8 C9 O1 114.7(12) . . ? C9 C10 C11 120.6(10) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C6 C11 C10 120.9(10) . . ? C6 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? O1 C12 C13 106.9(13) . . ? O1 C12 H12A 110.3 . . ? C13 C12 H12A 110.3 . . ? O1 C12 H12B 110.3 . . ? C13 C12 H12B 110.4 . . ? H12A C12 H12B 108.6 . . ? C14 C13 C12 118.8(14) . . ? C14 C13 H13A 107.6 . . ? C12 C13 H13A 107.6 . . ? C14 C13 H13B 107.6 . . ? C12 C13 H13B 107.6 . . ? H13A C13 H13B 107.0 . . ? C13 C14 C15 106.7(13) . . ? C13 C14 H14A 110.4 . . ? C15 C14 H14A 110.4 . . ? C13 C14 H14B 110.4 . . ? C15 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? 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 N1 Ag N1 C5 10.7(9) 2_556 . . . ? N1 Ag N1 N2 -170.7(6) 2_556 . . . ? C5 N1 N2 C3 0.7(9) . . . . ? Ag N1 N2 C3 -178.3(5) . . . . ? N1 N2 C3 C4 -0.6(10) . . . . ? N1 N2 C3 C6 -179.1(7) . . . . ? N2 C3 C4 C5 0.2(10) . . . . ? C6 C3 C4 C5 178.5(9) . . . . ? N2 N1 C5 C4 -0.6(11) . . . . ? Ag N1 C5 C4 178.2(6) . . . . ? C3 C4 C5 N1 0.3(12) . . . . ? N2 C3 C6 C11 -172.6(8) . . . . ? C4 C3 C6 C11 9.3(15) . . . . ? N2 C3 C6 C7 8.0(13) . . . . ? C4 C3 C6 C7 -170.1(10) . . . . ? C11 C6 C7 C8 -3.4(14) . . . . ? C3 C6 C7 C8 176.0(9) . . . . ? C6 C7 C8 C9 4.3(15) . . . . ? C7 C8 C9 C10 -1.6(16) . . . . ? C7 C8 C9 O1 178.4(9) . . . . ? C12 O1 C9 C10 -0.4(16) . . . . ? C12 O1 C9 C8 179.6(10) . . . . ? C8 C9 C10 C11 -2.0(15) . . . . ? O1 C9 C10 C11 178.0(9) . . . . ? C7 C6 C11 C10 0.0(13) . . . . ? C3 C6 C11 C10 -179.5(8) . . . . ? C9 C10 C11 C6 2.8(15) . . . . ? C9 O1 C12 C13 -170.7(11) . . . . ? O1 C12 C13 C14 -58(2) . . . . ? C12 C13 C14 C15 -173.0(15) . . . . ? 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 N2 H2 O2 1.00 1.72 2.702(9) 166.8 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.038 _refine_diff_density_min -0.635 _refine_diff_density_rms 0.113