Carbonyl complexes of copper(i) stabilized by bridging fluorinated pyrazolates and halide ions.
Parasar, Devaborniny; Jayaratna, Naleen B.; Muñoz-Castro, Alvaro; Conway, Allison E.; Mykhailiuk, Pavel K.; Dias, H. V. Rasika; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6358–6371; doi:10.1039/c9dt00486f

data_7049452
_publ_section_title
;
 Carbonyl complexes of copper(i) stabilized by bridging fluorinated
 pyrazolates and halide ions.
;
_journal_issue                   19
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6358
_journal_page_last               6371
_journal_paper_doi               10.1039/c9dt00486f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'Br C24 Cl4 Cu4 F24 N8 O4, C8 H20 N'
_chemical_formula_sum            'C32 H20 Br Cl4 Cu4 F24 N9 O4'
_chemical_formula_weight         1526.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-31 deposited with the CCDC.    2019-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.807(3)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   51.263(5)
_cell_length_b                   16.7952(15)
_cell_length_c                   17.4829(15)
_cell_measurement_reflns_used    9275
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.50
_cell_measurement_theta_min      3.08
_cell_volume                     14999(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0437
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       73
_diffrn_reflns_limit_h_min       -73
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            104971
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.541
_diffrn_reflns_theta_min         2.693
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.829
_exptl_absorpt_correction_T_max  0.3368
_exptl_absorpt_correction_T_min  0.2521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0824 before and 0.0574 after correction. The Ratio of minimum to maximum transmission is 0.7485. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.028
_exptl_crystal_description       rods
_exptl_crystal_F_000             8904
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.718
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1117
_refine_ls_number_reflns         22904
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0333P)^2^+30.1669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17425
_reflns_number_total             22904
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00486f2.cif
_cod_data_source_block           rad630_0m_a
_cod_depositor_comments
'Adding full bibliography for 7049446--7049452.cif.'
_cod_database_code               7049452
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.602
_shelx_estimated_absorpt_t_min   0.397
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F10-F11 \\sim F10-F12 \\sim F11-F12 \\sim F12A-F11A \\sim F12A-F10A \\sim
F11A-F10A
 with sigma of 0.04
 C10-F10 \\sim C10-F11 \\sim C10-F12 \\sim C10-F12A \\sim C10-F11A \\sim
C10-F10A
 with sigma of 0.02
 F31-F32 \\sim F31-F33 \\sim F32-F33 \\sim F32A-F33A \\sim F32A-F31A \\sim
F33A-F31A
 with sigma of 0.04
 C29-F31 \\sim C29-F32 \\sim C29-F33 \\sim C29-F32A \\sim C29-F33A \\sim
C29-F31A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F12) \\sim Ueq, Uanis(F12A) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F10A)
\\sim Ueq, Uanis(F11) \\sim Ueq, Uanis(F11A) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
Uanis(F33A) \\sim Ueq, Uanis(F33) \\sim Ueq, Uanis(F31A) \\sim Ueq, Uanis(F31)
\\sim Ueq, Uanis(F32A) \\sim Ueq, Uanis(F32) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.005
Uanis(C46) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(F3) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq: with sigma of
0.008 and sigma for terminal atoms of 0.008
4. Others
 Sof(F12A)=Sof(F11A)=Sof(F10A)=1-FVAR(1)
 Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(F32A)=Sof(F33A)=Sof(F31A)=1-FVAR(2)
 Sof(F31)=Sof(F32)=Sof(F33)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,
 H45B), C47(H47A,H47B)
5.b Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C48(H48A,H48B,H48C)
;
_shelx_res_checksum              74910
_olex2_submission_special_instructions 'No special instructions were received'