Synthesis and characterisation of copper(I) complexes with relevance to intramolecular Ullmann <i>O</i>,<i>S</i>-arylation.
Jin, Xiaodong; Nguyen, Bao-Nguyen T; Davies, Robert P.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 12554–12559; doi:10.1039/d4dt01418a

data_7716607
_publ_section_title
;
 Synthesis and characterisation of copper(I) complexes with relevance to
 intramolecular Ullmann <i>O</i>,<i>S</i>-arylation.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12554
_journal_page_last               12559
_journal_paper_doi               10.1039/d4dt01418a
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C56 H48 Br4 Cu4 N8 S4, 0.5(C7 H8)'
_chemical_formula_sum            'C59.5 H52 Br4 Cu4 N8 S4'
_chemical_formula_weight         1581.13
_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   mixed
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-04-18 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                75.376(4)
_cell_angle_beta                 81.788(4)
_cell_angle_gamma                81.693(3)
_cell_formula_units_Z            2
_cell_length_a                   10.3465(5)
_cell_length_b                   13.9442(4)
_cell_length_c                   21.4846(10)
_cell_measurement_reflns_used    5171
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      73.6760
_cell_measurement_theta_min      4.2740
_cell_volume                     2949.4(2)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 10.4115
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16916
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.736
_diffrn_reflns_theta_min         3.480
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.491
_exptl_absorpt_correction_T_max  0.856
_exptl_absorpt_correction_T_min  0.272
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       plates
_exptl_crystal_F_000             1570
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         11244
_refine_ls_number_restraints     444
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0665
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0409P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1040
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8496
_reflns_number_total             11244
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01418a2.cif
_cod_data_source_block           Cu4_3b-prime4
_cod_depositor_comments
'Adding full bibliography for 7716605--7716610.cif.'
_cod_original_formula_sum        'C59.50 H52 Br4 Cu4 N8 S4'
_cod_database_code               7716607
_shelx_shelxl_version_number     2019/3
_shelx_res_checksum              67668
_shelx_hkl_checksum              66918