Synthesis, structure and photophysical properties of two tetranuclear copper(I) iodide complexes based on acetylpyridine and diphosphine mixed ligands
Cao, Bing-Jun; Li, Ran; Huang, Xi-He; Acta Crystallographica Section C 77 (2021) 61–67; doi:10.1107/S2053229620016745

data_2022307
_publ_section_title
;
 Synthesis, structure and photophysical properties of two tetranuclear
 copper(I) iodide complexes based on acetylpyridine and diphosphine mixed
 ligands
;
_journal_coeditor_code           KY3202
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              61
_journal_page_last               67
_journal_paper_doi               10.1107/S2053229620016745
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac
'[Cu4 I4 (C6 H7 N O)2 (C27 H26 P2)2], 2C H2 Cl2'
_chemical_formula_moiety         'C68 H66 Cu4 I4 N2 O2 P4, 2C H2 Cl2'
_chemical_formula_sum            'C70 H70 Cl4 Cu4 I4 N2 O2 P4'
_chemical_formula_weight         1998.72
_chemical_name_systematic
;[\m~2~-1,3-Bis(diphenylphosphanyl)propane-\k^2^<i>P</i>:<i>P</i>']di-\m~3~-iodido-di-\m~2~-iodido-[1-(pyridin-3-yl)ethan-1-one-\k<i>N</i>]tetracopper(I)
dichloromethane disolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
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_cell_angle_beta                 86.30(3)
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_cell_length_b                   12.443(3)
_cell_length_c                   13.060(3)
_cell_measurement_reflns_used    6740
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      3.00
_cell_volume                     1915.1(7)
_computing_cell_refinement
;
RAPID AUTO (Rigaku, 1998)
;
_computing_data_collection
;
RAPID AUTO (Rigaku, 1998)
;
_computing_data_reduction
;
RAPID AUTO (Rigaku, 1998)
;
_computing_molecular_graphics
;
SHELXTL/PC (Sheldrick, 1993)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-axis RAPID'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0806
_diffrn_reflns_av_unetI/netI     0.0947
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15188
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         3.004
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.974
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3629
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(RAPID AUTO; Rigaku, 1998)
;
_exptl_crystal_colour            'yellowish green'
_exptl_crystal_density_diffrn    1.733
_exptl_crystal_description       block
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_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.092
_refine_diff_density_min         -0.642
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0843
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0453P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1214
_reflns_number_gt                4522
_reflns_number_total             6740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ky3202sup1.cif
_cod_data_source_block           CuL3
_cod_depositor_comments
'Adding full bibliography for 2022307--2022308.cif.'
_cod_original_cell_volume        1915.0(7)
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_cod_database_fobs_code          2022307
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