Rigidochromism of tetranuclear Cu(I)-pyrazolate macrocycles: steric crowding with trifluoromethyl groups.
Rajagopal, Shinaj K.; Zeller, Matthias; Savikhin, Sergei; Slipchenko, Lyudmila V.; Wei, Alexander; Chemical communications (Cambridge, England) 60 (2024) 11307–11310; doi:10.1039/d4cc04259j

data_7133719
_publ_section_title
;
 Rigidochromism of tetranuclear Cu(I)-pyrazolate macrocycles: steric
 crowding with trifluoromethyl groups.
;
_journal_issue                   80
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              11307
_journal_page_last               11310
_journal_paper_doi               10.1039/d4cc04259j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_sum            'C48 H72 Cu4 F12 N8'
_chemical_formula_weight         1243.29
_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
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2kk7zc
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-07-11 deposited with the CCDC.	2024-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.96(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.809(4)
_cell_length_b                   26.109(10)
_cell_length_c                   20.432(7)
_cell_measurement_reflns_used    9751
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      33.0090
_cell_measurement_theta_min      2.4218
_cell_volume                     5696(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_computing_data_collection       'Apex4 v2022.10-0 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_structure_refinement
;  
SHELXL-2019/2 (Sheldrick, 2015a, 2019), 
SHELXLE Rev1541 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015b)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type
'PhotonII charge-integrating pixel array (CPAD)'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device       'three circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS D8 Quest'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'Triumph curved graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            82366
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.178
_diffrn_reflns_theta_min         2.018
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    1.551
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.380
_exptl_crystal_size_min          0.310
_refine_diff_density_max         1.137
_refine_diff_density_min         -1.191
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1099
_refine_ls_number_reflns         20516
_refine_ls_number_restraints     2368
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0636P)^2^+2.3683P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1343
_refine_ls_wR_factor_ref         0.1512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13341
_reflns_number_total             20516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04259j2.cif
_cod_data_source_block           SKR_CF3_CPT_200_2_0m
_cod_depositor_comments
'Adding full bibliography for 7133719--7133720.cif.'
_cod_original_cell_volume        5696(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7133719
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.523
_shelx_estimated_absorpt_t_max   0.645
_shelx_res_checksum              86585
_shelx_hkl_checksum              76290