Relativistic Modulation of Supramolecular Halogen/Copper Interactions and Phosphorescence in Cu(I) Pyrazolate Cyclotrimers
Lu, Zhou; Vanga, Mukundam; Li, Shan; Adebanjo, Joseph; Patterson, Monika; Dias, Rasika; Omary, Mohammad; Dalton Transactions  (2023) –; doi:10.1039/D2DT03725D

data_7711928
_publ_section_title
;
 Relativistic Modulation of Supramolecular Halogen/Copper Interactions and
 Phosphorescence in Cu(I) Pyrazolate Cyclotrimers
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT03725D
_journal_year                    2023
_chemical_formula_moiety         'C15 Cu3 F18 I3 N6'
_chemical_formula_sum            'C15 Cu3 F18 I3 N6'
_chemical_formula_weight         1177.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_primary     dual
_audit_creation_date             2022-07-29
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-30 deposited with the CCDC.	2022-12-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.717(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2314(5)
_cell_length_b                   14.3123(7)
_cell_length_c                   20.1811(10)
_cell_measurement_reflns_used    9606
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.64
_cell_volume                     2642.2(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'Photon 100 CMOS'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '0.3\ \w and 0.3\ \f scans'
_diffrn_radiation_collimation    '0.6 mm double-pinhole'
_diffrn_radiation_detector       'Photon 100 CMOS'
_diffrn_radiation_monochromator  'curved graphite'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            57828
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.587
_diffrn_reflns_theta_min         2.570
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_type              'KFF MO-2KC-90'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.047
_exptl_absorpt_correction_T_max  0.2125
_exptl_absorpt_correction_T_min  0.1441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1042 before and 0.0667 after correction.
The Ratio of minimum to maximum transmission is 0.6781.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.960
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_refine_diff_density_max         3.382
_refine_diff_density_min         -1.883
_refine_diff_density_rms         0.305
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0625
_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^)+145.6139P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7258
_reflns_number_total             8101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt03725d2.cif
_cod_data_source_block           rad818_0m_c
_cod_database_code               7711928
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.393
_shelx_estimated_absorpt_t_min   0.292
_olex2_refinement_description
;
;
_shelx_res_checksum              12523
_shelx_hkl_checksum              5688
_olex2_submission_special_instructions 'No special instructions were received'