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_7049451
_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         'C17 H3 Cu2 F18 N6 O2, C8 H20 N'
_chemical_formula_sum            'C25 H23 Cu2 F18 N7 O2'
_chemical_formula_weight         922.58
_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                 115.266(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.7152(18)
_cell_length_b                   10.5333(5)
_cell_length_c                   18.8804(9)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.93
_cell_volume                     6783.0(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      100.19
_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  0.0251
_diffrn_reflns_av_unetI/netI     0.0185
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37162
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.541
_diffrn_reflns_theta_min         2.928
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.391
_exptl_absorpt_correction_T_max  0.3334
_exptl_absorpt_correction_T_min  0.2842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0777 before and 0.0512 after correction. The Ratio of minimum to maximum transmission is 0.8524. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.807
_exptl_crystal_description       block
_exptl_crystal_F_000             3664
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     531
_refine_ls_number_reflns         7805
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0269P)^2^+18.5334P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0754
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6884
_reflns_number_total             7805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00486f2.cif
_cod_data_source_block           rad383_0m_a
_cod_depositor_comments
'Adding full bibliography for 7049446--7049452.cif.'
_cod_database_code               7049451
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.873
_shelx_estimated_absorpt_t_min   0.759
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N7-C18 \\sim N7-C18A \\sim N7-C24A \\sim N7-C24 \\sim N7-C22 \\sim N7-C20
 with sigma of 0.005
 C21-C20 \\sim C23-C22 \\sim C25-C24 \\sim C25A-C24A \\sim C19A-C18A \\sim
C19-C18
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C18 \\sim C18A \\sim C19A \\sim C19 \\sim C24 \\sim C24A \\sim C25 \\sim C25A
\\sim C23 \\sim C21: within 1.7A with sigma of 0.008 and sigma for terminal
atoms of 0.008
Uanis(C19A) \\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19)
\\sim Ueq, Uanis(C24A) \\sim Ueq, Uanis(C25) \\sim Ueq, Uanis(C25A) \\sim Ueq,
Uanis(C24) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of
0.05 and sigma for terminal atoms of 0.05
Uanis(F10) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.008
4. Others
 Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=FVAR(1)
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=1-FVAR(2)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C20(H20A,H20B), C22(H22A,H22B), C24(H24A,H24B), C24A(H24C,
 H24D), C18A(H18C,H18D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C12(H12)
5.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C25(H25A,H25B,
 H25C), C25A(H25D,H25E,H25F), C19A(H19D,H19E,H19F)
;
_shelx_res_checksum              42254
_olex2_submission_special_instructions 'No special instructions were received'