Coinage metal metallacycles involving a fluorinated 3,5-diarylpyrazolate
Lakhi, Jaspreet S.; Patterson, Monika R.; Dias, H. V. Rasika; New Journal of Chemistry 44 (2020) 14814–14822; doi:10.1039/D0NJ03744C

data_7059859
_publ_section_title
;
 Coinage metal metallacycles involving a fluorinated 3,5-diarylpyrazolate
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14814
_journal_page_last               14822
_journal_paper_doi               10.1039/D0NJ03744C
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C57 H21 Ag3 F36 N6, C H2 Cl2'
_chemical_formula_sum            'C58 H23 Ag3 Cl2 F36 N6'
_chemical_formula_weight         1882.33
_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             2020-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-06-24 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                89.287(2)
_cell_angle_beta                 85.728(2)
_cell_angle_gamma                87.428(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6941(5)
_cell_length_b                   15.8573(8)
_cell_length_c                   26.1433(13)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.92
_cell_volume                     3590.5(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      299.06
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker D8 Quest with a Photon 100 CMOS detector'
_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  0.0332
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            37199
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.884
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.019
_exptl_absorpt_correction_T_max  0.3352
_exptl_absorpt_correction_T_min  0.2863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0846 before and 0.0373 after correction. The Ratio of minimum to maximum transmission is 0.8541. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.741
_exptl_crystal_description       block
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.748
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1170
_refine_ls_number_reflns         14836
_refine_ls_number_restraints     1905
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0615
_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^)+(0.1079P)^2^+4.4005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1723
_refine_ls_wR_factor_ref         0.1945
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9765
_reflns_number_total             14836
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03744c2.cif
_cod_data_source_block           rad378_0m_a
_cod_depositor_comments
'Adding full bibliography for 7059858--7059861.cif.'
_cod_database_code               7059859
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.830
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 Cl1-C58 = Cl2-C58
 1.7602 with sigma of 0.002
 Cl1-Cl2
 2.9338 with sigma of 0.004
 F13-C29 \\sim F14-C29 \\sim F15-C29 \\sim F16-C30 \\sim F17A-C30 \\sim F17-C30
\\sim F18A-C30 \\sim F18-
 C30 \\sim F16A-C30 \\sim F19A-C37 \\sim F20-C37 \\sim F20A-C37 \\sim F21-C37
\\sim F21A-C37 \\sim F19-C37
 \\sim F30-C49 \\sim F29-C49 \\sim F28-C49 \\sim F25A-C48 \\sim F27-C48 \\sim
F27A-C48 \\sim F26-C48 \\sim F26A-
 C48 \\sim F25-C48 \\sim F31-C56 \\sim F32A-C56 \\sim F32-C56 \\sim F33A-C56
\\sim F33-C56 \\sim F31A-C56 ~
 F34-C57 \\sim F35-C57 \\sim F36-C57 \\sim F1A-C10 \\sim F1-C10 \\sim F2-C10
\\sim F2A-C10 \\sim F3-C10 ~
 F3A-C10 \\sim F6-C11 \\sim F4A-C11 \\sim F4-C11 \\sim F5A-C11 \\sim F5-C11
\\sim F6A-C11 \\sim F8-C18 ~
 F8A-C18 \\sim F9-C18 \\sim F9A-C18 \\sim F7-C18 \\sim F7A-C18 \\sim F12-C19
\\sim F11-C19 \\sim F10-C19
 with sigma of 0.008
 F24-C38 \\sim F23-C38 \\sim F22-C38
 with sigma of 0.005
 F23A-C38 \\sim F23-C38 \\sim F24A-C38 \\sim F24-C38 \\sim F22A-C38 \\sim
F22-C38
 with sigma of 0.008
 F22-F23 \\sim F22-F24 \\sim F23-F24 \\sim F22A-F23A \\sim F22A-F24A \\sim
F23A-F24A
 with sigma of 0.01
3. Rigid bond restraints
 F22, F23, F24, F22A, F23A, F24A
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 Cl1, Cl2
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.008
 C58
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 0.008
4. Uiso/Uaniso restraints and constraints
F22 \\sim F23 \\sim F24 \\sim F22A \\sim F23A \\sim F24A: within 1.7A with
sigma of 0.008 and sigma for terminal atoms of 0.008
Cl1 \\sim Cl2: within 1.7A with sigma of 0.008 and sigma for terminal atoms of
0.008
C58: within 1.7A with sigma of 0.008 and sigma for terminal atoms of 0.008
Uanis(Cl2) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(Cl1) \\sim Ueq, Uanis(C29)
\\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C58) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
Uanis(F10) \\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F13)
\\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq, Uanis(F28) \\sim Ueq,
Uanis(F29) \\sim Ueq, Uanis(F30) \\sim Ueq, Uanis(F34) \\sim Ueq, Uanis(F35)
\\sim Ueq, Uanis(F36) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq,
Uanis(F3) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim
Ueq, Uanis(F7) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F16)
\\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19) \\sim Ueq,
Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F22) \\sim Ueq, Uanis(F23)
\\sim Ueq, Uanis(F24) \\sim Ueq, Uanis(F25) \\sim Ueq, Uanis(F26) \\sim Ueq,
Uanis(F27) \\sim Ueq, Uanis(F31) \\sim Ueq, Uanis(F32) \\sim Ueq, Uanis(F33)
\\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq,
Uanis(F4A) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F7A)
\\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(F16A) \\sim Ueq,
Uanis(F17A) \\sim Ueq, Uanis(F18A) \\sim Ueq, Uanis(F19A) \\sim Ueq,
Uanis(F20A) \\sim Ueq, Uanis(F21A) \\sim Ueq, Uanis(F22A) \\sim Ueq,
Uanis(F23A) \\sim Ueq, Uanis(F24A) \\sim Ueq, Uanis(F25A) \\sim Ueq,
Uanis(F26A) \\sim Ueq, Uanis(F27A) \\sim Ueq, Uanis(F31A) \\sim Ueq,
Uanis(F32A) \\sim Ueq, Uanis(F33A) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.008
5. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F4)=Sof(F5)=Sof(F6)=FVAR(1)
 Sof(F31A)=Sof(F32A)=Sof(F33A)=1-FVAR(2)
 Sof(F31)=Sof(F32)=Sof(F33)=FVAR(2)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=1-FVAR(3)
 Sof(F1)=Sof(F2)=Sof(F3)=FVAR(3)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(4)
 Sof(F7)=Sof(F8)=Sof(F9)=FVAR(4)
 Sof(F25A)=Sof(F26A)=Sof(F27A)=1-FVAR(5)
 Sof(F25)=Sof(F26)=Sof(F27)=FVAR(5)
 Sof(F19A)=Sof(F20A)=Sof(F21A)=1-FVAR(6)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(6)
 Sof(F16A)=Sof(F17A)=Sof(F18A)=1-FVAR(7)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(7)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(8)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(8)
6.a Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C7(H7), C9(H9), C13(H13), C15(H15), C17(H17), C21(H21),
 C24(H24), C26(H26), C28(H28), C32(H32), C34(H34), C36(H36), C40(H40), C43(H43),
  C45(H45), C47(H47), C51(H51), C53(H53), C55(H55)
;
_shelx_res_checksum              15598
_shelx_fab_checksum              92245
_olex2_submission_special_instructions 'No special instructions were received'