Structural and photophysical characterization of mono- and binuclear Cu(i) complexes based on carbohydrazones: a combined experimental and computational study
Gholivand, Khodayar; Farshadfer, Kaveh; Roe, S. Mark; Gholami, Akram; Esrafili, Mehdi D.; CrystEngComm 18 (2016) 2873–; doi:10.1039/C5CE02208H

data_7224588
_publ_section_title
;
 Structural and photophysical characterization of mono- and binuclear
 Cu(i) complexes based on carbohydrazones: a combined experimental and
 computational study
;
_journal_issue                   16
_journal_name_full               CrystEngComm
_journal_page_first              2873
_journal_paper_doi               10.1039/C5CE02208H
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C58 H48 Cl2 Cu2 N6 O2 P2 S2'
_chemical_formula_sum            'C58 H48 Cl2 Cu2 N6 O2 P2 S2'
_chemical_formula_weight         1185.06
_chemical_name_common            Cp1
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2016-02-11 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.412(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.3680(11)
_cell_length_b                   14.5156(9)
_cell_length_c                   18.5708(9)
_cell_measurement_reflns_used    4932
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      28.8460
_cell_measurement_theta_min      4.0390
_cell_volume                     5553.0(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.852
_diffrn_measurement_details
;
  1 omega  -35.00   53.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -16.2858   38.0000  150.0000 88

  2 omega  -88.00  -35.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -16.2858 -178.0000  150.0000 53

  3 omega  -88.00  -35.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -16.2858 -178.0000  -60.0000 53

  4 omega  -30.00   45.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -16.2858   57.0000    0.0000 75

  5 omega   -3.00   46.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       17.0670  -99.0000   90.0000 49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0297198000
_diffrn_orient_matrix_UB_12      0.0239707000
_diffrn_orient_matrix_UB_13      -0.0044737000
_diffrn_orient_matrix_UB_21      0.0132482000
_diffrn_orient_matrix_UB_22      0.0385171000
_diffrn_orient_matrix_UB_23      -0.0141529000
_diffrn_orient_matrix_UB_31      -0.0113580000
_diffrn_orient_matrix_UB_32      -0.0178950000
_diffrn_orient_matrix_UB_33      -0.0367799000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.852
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            18779
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.557
_diffrn_reflns_theta_min         3.579
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          1.0
_exptl_crystal_size_min          0.6
_refine_diff_density_max         1.264
_refine_diff_density_min         -1.176
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6619
_refine_ls_number_restraints     303
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0940P)^2^+8.7920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1700
_refine_ls_wR_factor_ref         0.1830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4955
_reflns_number_total             6619
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02208h2.cif
_cod_data_source_block           cucl545
_cod_depositor_comments
'Adding full bibliography for 7224588--7224592.cif.'
_cod_database_code               7224588
_chemical_oxdiff_formula         C29H24Cl1N3O1P1S1Cu1
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Rigid body (RIGU) restrains
 Cu1, Cl2, P1, Cl1, N1, C18, C12, C24, C5, C1, C19, C23, C17, C13, C25, C29,
 H5, C4, H1, C2, H19, C20, H23, C22, H17, C16, H13, C14, H25, C26, H29, C28, C3,
  H4, H2, H20, C21, H22, H16, C15, H14, C27, H26, H28, C6, H21, H15, H27, N2,
 H6, N3, H3, C7, O1, C8, S1, C9, C11, C10, H11, H10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C9(H9), C10(H10), C11(H11),
 C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'