Mixed ligand complexes of silver(i) supported by highly fluorinated pyrazolates, and chelating and bridging N-heterocycles
Dias, H. V. Rasika; Palehepitiya Gamage, Chammi S.; Jayaratna, Naleen B.; Hettiarachchi, Champika V.; New Journal of Chemistry 44 (2020) 17079–17087; doi:10.1039/D0NJ04007J

data_7059980
_publ_section_title
;
 Mixed ligand complexes of silver(i) supported by highly fluorinated
 pyrazolates, and chelating and bridging N-heterocycles
;
_journal_issue                   39
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17079
_journal_page_last               17087
_journal_paper_doi               10.1039/D0NJ04007J
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C56 H28 Ag4 F24 N14, C7 H8'
_chemical_formula_sum            'C63 H36 Ag4 F24 N14'
_chemical_formula_weight         1876.54
_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     direct
_audit_creation_date             2020-09-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-11 deposited with the CCDC.	2020-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                92.125(5)
_cell_angle_beta                 96.546(6)
_cell_angle_gamma                103.553(11)
_cell_formula_units_Z            2
_cell_length_a                   12.1451(13)
_cell_length_b                   13.5207(14)
_cell_length_c                   20.327(3)
_cell_measurement_reflns_used    7974
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.49
_cell_volume                     3216.8(7)
_computing_cell_refinement       'SAINT v7.06A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v7.06A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0293
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30094
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.275
_diffrn_reflns_theta_min         1.739
_exptl_absorpt_coefficient_mu    1.324
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS v.2.10 (Bruker,2003) was used for absorption correction. R(int) was 0.0429 before and 0.0289 after correction. The Ratio of minimum to maximum transmission is 0.7208. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.937
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.381
_refine_diff_density_min         -0.653
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1038
_refine_ls_number_reflns         15308
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+0.4926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.0973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12705
_reflns_number_total             15308
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj04007j2.cif
_cod_data_source_block           dias46s
_cod_depositor_comments
'Adding full bibliography for 7059979--7059984.cif.'
_cod_database_code               7059980
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.890
_shelx_estimated_absorpt_t_min   0.725
_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. Restrained distances
 F20A-C43 \\sim F20-C43 \\sim F19A-C43 \\sim F19-C43 \\sim F21A-C43 \\sim
F21-C43
 with sigma of 0.01
3. Others
 Fixed Sof: F19(0.459) F20(0.459) F21(0.459) F19A(0.541) F20A(0.541)
 F21A(0.541) C64(0.5) C65(0.5) H65(0.5) C66(0.5) H66(0.5) C67(0.5) H67(0.5)
 C68(0.5) H68(0.5) C69(0.5) H69(0.5) C70(0.5) H70A(0.5) H70B(0.5) H70C(0.5)
 C57(0.5) C58(0.5) H58(0.5) C59(0.5) H59(0.5) C60(0.5) H60(0.5) C61(0.5)
 H61(0.5) C62(0.5) H62(0.5) C63(0.5) H63A(0.5) H63B(0.5) H63C(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C11(H11), C12(H12), C13(H13), C16(H16), C17(H17), C18(H18),
 C20(H20), C21(H21), C23(H23), C24(H24), C25(H25), C28(H28), C29(H29), C30(H30),
  C32(H32), C33(H33), C36(H36), C41(H41), C45(H45), C46(H46), C47(H47),
 C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C65(H65), C66(H66), C67(H67),
  C68(H68), C69(H69), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62)
4.b Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              45644
_olex2_submission_special_instructions 'No special instructions were received'