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_7133720
_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      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
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2kk83j
_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                104.128(12)
_cell_angle_beta                 95.625(12)
_cell_angle_gamma                95.573(10)
_cell_formula_units_Z            8
_cell_length_a                   10.7542(15)
_cell_length_b                   33.091(5)
_cell_length_c                   33.101(6)
_cell_measurement_reflns_used    9735
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.0961
_cell_measurement_theta_min      2.7778
_cell_volume                     11278(3)
_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 Rev1506 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015b)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type
'PhotonII charge-integrating pixel array (CPAD)'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0398
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       50
_diffrn_reflns_limit_k_min       -50
_diffrn_reflns_limit_l_max       50
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            465628
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.196
_diffrn_reflns_theta_min         1.944
_diffrn_source                   'fine focus sealed tube X-ray source'
_diffrn_source_current           '30 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    1.567
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6844
_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    1.464
_exptl_crystal_description       block
_exptl_crystal_F_000             5120
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.170
_refine_diff_density_max         1.464
_refine_diff_density_min         -0.758
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2690
_refine_ls_number_reflns         86222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+2.1071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0734
_reflns_Friedel_coverage         0.000
_reflns_number_gt                78076
_reflns_number_total             86222
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc04259j2.cif
_cod_data_source_block           SKR_1_131_Cu4_CF3Py4_0m
_cod_depositor_comments
'Adding full bibliography for 7133719--7133720.cif.'
_cod_database_code               7133720
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.587
_shelx_estimated_absorpt_t_max   0.777
_shelx_res_checksum              2094
_shelx_hkl_checksum              85863