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_7701730
_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         'C52 H40 Ag N4, C30 H6 Ag5 F36 N12'
_chemical_formula_sum            'C82 H46 Ag6 F36 N16'
_chemical_formula_weight         2586.57
_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                79.6540(10)
_cell_angle_beta                 81.7590(10)
_cell_angle_gamma                87.1010(10)
_cell_formula_units_Z            4
_cell_length_a                   14.3696(5)
_cell_length_b                   16.7297(6)
_cell_length_c                   38.1790(13)
_cell_measurement_reflns_used    9844
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.222
_cell_volume                     8932.8(5)
_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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0613
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            138385
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.659
_diffrn_reflns_theta_min         1.432
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.419
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0887 before and 0.0453 after correction. The Ratio of minimum to maximum transmission is 0.8181. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_description       prism
_exptl_crystal_F_000             5024
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.951
_refine_diff_density_min         -1.254
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2529
_refine_ls_number_reflns         55006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0344P)^2^+7.4975P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0984
_reflns_Friedel_coverage         0.000
_reflns_number_gt                38738
_reflns_number_total             55006
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01355e2.cif
_cod_data_source_block           a_CCDC1
_cod_database_code               7701730
_shelxl_version_number           2014/6
_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:
 C2A(H2A), C5A(H5A), C6A(H6A), C9A(H9A), C16A(H16A), C17A(H17A), C18A(H18A),
 C19A(H19A), C20A(H20A), C22A(H22A), C23A(H23A), C24A(H24A), C25A(H25A),
 C26A(H26A), C28A(H28A), C31A(H31A), C32A(H32A), C35A(H35A), C42A(H42A),
 C43A(H43A), C44A(H44A), C45A(H45A), C46A(H46A), C48A(H48A), C49A(H49A),
 C50A(H50A), C51A(H51A), C52A(H52A), C2B(H2B), C5B(H5B), C6B(H6B), C9B(H9B),
 C16B(H16B), C17B(H17B), C18B(H18B), C19B(H19B), C20B(H20B), C22B(H22B),
 C23B(H23B), C24B(H24B), C25B(H25B), C26B(H26B), C28B(H28B), C31B(H31B),
 C32B(H32B), C35B(H35B), C42B(H42B), C43B(H43B), C44B(H44B), C45B(H45B),
 C46B(H46B), C48B(H48B), C49B(H49B), C50B(H50B), C51B(H51B), C52B(H52B),
 C54A(H54A), C57A(H57A), C60A(H60A), C63A(H63A), C66A(H66A), C69A(H69A),
 C54B(H54B), C57B(H57B), C60B(H60B), C63B(H63B), C66B(H66B), C69B(H69B)
2.b Idealised Me refined as rotating group:
 C13A(H13A,H13B,H13C), C14A(H14A,H14B,H14C), C39A(H39A,H39B,H39C), C40A(H40A,
 H40B,H40C), C13B(H13D,H13E,H13F), C14B(H14D,H14E,H14F), C39B(H39D,H39E,H39F),
 C40B(H40D,H40E,H40F)
;
_shelx_res_checksum              68067
_olex2_submission_special_instructions 'No special instructions were received'