Synthesis and structural characterization of hexa-μ~2~-chlorido-μ~4~-oxido-tetrakis{[4-(phenylethynyl)pyridine-κ<i>N</i>]copper(II)} dichloromethane monosolvate
Al Balushi, Rayya A.; Khan, Muhammad S.; Faizi, Md. Serajul Haque; Haque, Ashanul; Molloy, Kieran; Raithby, Paul R.; Acta Crystallographica Section E 77 (2021) 42–46; doi:10.1107/S2056989020015935

data_2243704
_publ_section_title
;
 Synthesis and structural characterization of
 hexa-\m~2~-chlorido-\m~4~-oxido-tetrakis{[4-(phenylethynyl)pyridine-\k<i>N</i>]copper(II)}
 dichloromethane monosolvate
;
_journal_coeditor_code           MW2170
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              42
_journal_page_last               46
_journal_paper_doi               10.1107/S2056989020015935
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac          '[Cu4 Cl6 O (C13 H9 N1)4], C H2 Cl2'
_chemical_formula_moiety         'C52 H36 Cl6 Cu4 N4 O, C H2 Cl2'
_chemical_formula_sum            'C53 H38 Cl8 Cu4 N4 O'
_chemical_formula_weight         1284.63
_chemical_name_systematic
'Hexa-\m~2~-chlorido-\m~4~-oxido-tetrakis{[4-(phenylethynyl)pyridine-\k<i>N</i>]copper(II)} dichloromethane monosolvate'
_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
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                105.0240(10)
_cell_angle_beta                 105.9350(10)
_cell_angle_gamma                102.9990(10)
_cell_formula_units_Z            2
_cell_length_a                   12.7166(2)
_cell_length_b                   14.4366(2)
_cell_length_c                   16.4038(3)
_cell_measurement_reflns_used    38646
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     2650.82(8)
_computing_cell_refinement
;
HKL SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Nonius, 1998)
;
_computing_data_reduction
;
HKL and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows  (Farrugia,
2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '274 2.0 degree images with \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0639
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            50117
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.557
_diffrn_reflns_theta_min         3.023
_exptl_absorpt_coefficient_mu    2.029
_exptl_absorpt_correction_T_max  0.572
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(Sortav; Blessing 1995)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.887
_refine_diff_density_min         -0.994
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         12164
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0564P)^2^+3.7541P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1267
_reflns_number_gt                8495
_reflns_number_total             12164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            mw2170sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2650.81(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2243704
_shelx_estimated_absorpt_t_min   0.751
_shelx_estimated_absorpt_t_max   0.793
_shelx_hkl_checksum              33551
_shelx_res_checksum              29754
_cod_database_fobs_code 2243704