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_7059861
_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 Cu3 F36 N6, 1.5(C7 H8)'
_chemical_formula_sum            'C67.5 H33 Cu3 F36 N6'
_chemical_formula_weight         1802.62
_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             2020-06-12
_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                107.382(2)
_cell_angle_beta                 91.600(2)
_cell_angle_gamma                98.226(2)
_cell_formula_units_Z            2
_cell_length_a                   8.4054(10)
_cell_length_b                   19.555(2)
_cell_length_c                   21.674(2)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      3.03
_cell_volume                     3355.4(6)
_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      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_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  0.0440
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            30015
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.827
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.091
_exptl_absorpt_correction_T_max  0.2092
_exptl_absorpt_correction_T_min  0.1677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0555 before and 0.0480 after correction. The Ratio of minimum to maximum transmission is 0.8016. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       needles
_exptl_crystal_F_000             1782
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.395
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1104
_refine_ls_number_reflns         13114
_refine_ls_number_restraints     327
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0864
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0988P)^2^+55.2301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2395
_refine_ls_wR_factor_ref         0.2592
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10366
_reflns_number_total             13114
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj03744c2.cif
_cod_data_source_block           rad539_0m_a
_cod_depositor_comments
'Adding full bibliography for 7059858--7059861.cif.'
_cod_original_cell_volume        3355.4(7)
_cod_original_formula_sum        'C67.50 H33 Cu3 F36 N6'
_cod_database_code               7059861
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.735
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9427(11)
 0.0573(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C1A-C1B
 1.51 with sigma of 0.02
 F10-F11 \\sim F10-F12 \\sim F11-F12 \\sim F11A-F12A \\sim F11A-F10A \\sim
F12A-F10A
 with sigma of 0.04
 C19-F10 \\sim C19-F11 \\sim C19-F12 \\sim C19-C16 \\sim C19-F11A \\sim
C19-F12A \\sim C19-F10A
 with sigma of 0.02
 C1B-C1C \\sim C1C-C1D \\sim C1D-C1E \\sim C1E-C1F \\sim C1F-C1G \\sim C1G-C1B
 with sigma of 0.02
 C1B-C1F \\sim C1B-C1D \\sim C1G-C1E \\sim C1C-C1G \\sim C1D-C1F \\sim C1C-C1E
 with sigma of 0.04
 C1A-C1G \\sim C1A-C1C
 with sigma of 0.04
4. Restrained planarity
 C1A, C1B, C1C, C1D, C1E, C1F, C1G
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C1A \\sim C1B \\sim C1C \\sim C1D \\sim C1E \\sim C1F \\sim C1G: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(F25) \\sim Ueq, Uanis(F20) \\sim Ueq: with sigma of 0.008 and sigma for
terminal atoms of 0.008
Uanis(F11A) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(F10)
\\sim Ueq, Uanis(F10A) \\sim Ueq, Uanis(F11) \\sim Ueq: with sigma of 0.008 and
sigma for terminal atoms of 0.008
Uanis(C1B) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
6. Rigid body (RIGU) restrains
 F10, F11, F12, C19, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F11A, F12A, F10A, C19, C16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, F28, F30, F29, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F29A, F28A, F30A, C49, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1A, C1B, C1C, C1D, C1E, C1F, C1G
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
7. Others
 Sof(F11A)=Sof(F12A)=Sof(F10A)=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(F29A)=Sof(F28A)=Sof(F30A)=1-FVAR(2)
 Sof(F28)=Sof(F29)=Sof(F30)=FVAR(2)
 Fixed Sof: C1A(0.5) H1AA(0.5) H1AB(0.5) H1AC(0.5) C1B(0.5) C1C(0.5) H1C(0.5)
 C1D(0.5) H1D(0.5) C1E(0.5) H1E(0.5) C1F(0.5) H1F(0.5) C1G(0.5) H1G(0.5)
8.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), C59(H59), C60(H60),
 C61(H61), C62(H62), C63(H63), C1C(H1C), C1D(H1D), C1E(H1E), C1F(H1F), C1G(H1G)
8.b Idealised Me refined as rotating group:
 C64(H64A,H64B,H64C), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              94414
_olex2_submission_special_instructions 'No special instructions were received'