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_7059860
_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 Au3 F36 N6'
_chemical_formula_sum            'C57 H21 Au3 F36 N6'
_chemical_formula_weight         2064.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-07-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2020-06-24 deposited with the CCDC.	2020-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.507(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3667(5)
_cell_length_b                   31.7232(19)
_cell_length_c                   25.7197(15)
_cell_measurement_reflns_used    9522
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.99
_cell_measurement_theta_min      3.02
_cell_volume                     6824.1(7)
_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      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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  0.0345
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            89629
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.027
_diffrn_reflns_theta_min         2.847
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.573
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.4876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1061 before and 0.0524 after correction. The Ratio of minimum to maximum transmission is 0.6536. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_description       plates
_exptl_crystal_F_000             3864
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.845
_refine_diff_density_min         -1.656
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1031
_refine_ls_number_reflns         19862
_refine_ls_number_restraints     366
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+34.5925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0664
_refine_ls_wR_factor_ref         0.0702
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17064
_reflns_number_total             19862
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03744c2.cif
_cod_data_source_block           rad533_0m_a_sq
_cod_depositor_comments
'Adding full bibliography for 7059858--7059861.cif.'
_cod_database_code               7059860
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.589
_shelx_estimated_absorpt_t_min   0.260
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 F21A-F20A \\sim F20-F21 \\sim F20A-F19A
 with sigma of 0.04
 C37-F21A \\sim C37-F20 \\sim C37-F20A \\sim C37-F19 \\sim C37-F19A \\sim
C37-F21 \\sim C37-C33
 with sigma of 0.02
 F16-F17 \\sim F16-F18 \\sim F17-F18 \\sim F16A-F18A \\sim F16A-F17A \\sim
F18A-F17A
 with sigma of 0.04
 C30-F16 \\sim C30-F17 \\sim C30-F18 \\sim C30-C27 \\sim C30-F16A \\sim
C30-F18A \\sim C30-F17A
 with sigma of 0.02
 F13-F14 \\sim F13-F15 \\sim F14-F15 \\sim F13A-F15A \\sim F13A-F14A \\sim
F15A-F14A
 with sigma of 0.04
 C29-F13 \\sim C29-F14 \\sim C29-F15 \\sim C29-C25 \\sim C29-F13A \\sim
C29-F15A \\sim C29-F14A
 with sigma of 0.02
 F31-F32 \\sim F31-F33 \\sim F32-F33 \\sim F33A-F32A \\sim F33A-F31A \\sim
F32A-F31A
 with sigma of 0.04
 C56-F31 \\sim C56-F32 \\sim C56-F33 \\sim C56-C52 \\sim C56-F33A \\sim
C56-F32A \\sim C56-F31A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F30) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005
4. Rigid body (RIGU) restrains
 F19, F20, F21, C33, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, F19A, F21A, F20A, C33, C37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F16, C30, F17, F18, C27
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C27, C30, F16A, F18A, F17A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F13, C25, C29, F14, F15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C25, C29, F13A, F14A, F15A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C52, C56, F32, F33, F31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C52, F33A, F31A, F32A, C56
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(F19A)=Sof(F21A)=Sof(F20A)=1-FVAR(1)
 Sof(F19)=Sof(F20)=Sof(F21)=FVAR(1)
 Sof(F16A)=Sof(F18A)=Sof(F17A)=1-FVAR(2)
 Sof(F16)=Sof(F17)=Sof(F18)=FVAR(2)
 Sof(F13A)=Sof(F15A)=Sof(F14A)=1-FVAR(3)
 Sof(F13)=Sof(F14)=Sof(F15)=FVAR(3)
 Sof(F33A)=Sof(F32A)=Sof(F31A)=1-FVAR(4)
 Sof(F31)=Sof(F32)=Sof(F33)=FVAR(4)
6.a 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              71627
_shelx_fab_checksum              80373
_olex2_submission_special_instructions 'No special instructions were received'