Synthesis, structures and luminescence of multinuclear silver(i) pyrazolate adducts with 1,10-phenanthroline derivatives.
Titov, Aleksei A.; Filippov, Oleg A.; Smol'yakov, Alexander F.; Averin, Aleksey A.; Shubina, Elena S.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8410–8417; doi:10.1039/c9dt01355e

data_7701729
_publ_section_title
;
 Synthesis, structures and luminescence of multinuclear silver(i)
 pyrazolate adducts with 1,10-phenanthroline derivatives.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8410
_journal_page_last               8417
_journal_paper_doi               10.1039/c9dt01355e
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C48 H28 Ag4 F24 N12'
_chemical_formula_sum            'C48 H28 Ag4 F24 N12'
_chemical_formula_weight         1660.30
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-29 deposited with the CCDC.	2019-05-07 downloaded from the CCDC.
;
_cell_angle_alpha                65.492(3)
_cell_angle_beta                 85.582(3)
_cell_angle_gamma                70.097(3)
_cell_formula_units_Z            1
_cell_length_a                   10.762(2)
_cell_length_b                   11.734(2)
_cell_length_c                   12.469(2)
_cell_measurement_reflns_used    9085
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.09
_cell_measurement_theta_min      2.48
_cell_volume                     1343.4(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0375
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20802
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.152
_diffrn_reflns_theta_min         1.800
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.569
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.1131 before and 0.0461 after correction. The Ratio of minimum to maximum transmission is 0.8132. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.052
_exptl_crystal_description       prism
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.018
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         7207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.7867P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0706
_refine_ls_wR_factor_ref         0.0767
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5890
_reflns_number_total             7207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01355e2.cif
_cod_data_source_block           a
_cod_database_code               7701729
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.859
_shelx_estimated_absorpt_t_min   0.650
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C14(H14), C15(H15), C9(H9), C5(H5), C8(H8), C11(H11), C12(H12)
2.b Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              18646
_olex2_submission_special_instructions 'No special instructions were received'