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_7224592
_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 Br2 Cu2 N6 O2 P2 S2, C4 H6 N2'
_chemical_formula_sum            'C62 H54 Br2 Cu2 N8 O2 P2 S2'
_chemical_formula_weight         1356.08
_chemical_name_common            Cp2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-18
_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                69.313(11)
_cell_angle_beta                 83.252(9)
_cell_angle_gamma                72.076(10)
_cell_formula_units_Z            1
_cell_length_a                   8.5296(9)
_cell_length_b                   13.6245(18)
_cell_length_c                   14.4843(17)
_cell_measurement_reflns_used    2219
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      70.7690
_cell_measurement_theta_min      3.9530
_cell_volume                     1498.2(3)
_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 0.979
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_details
;
  1 omega  -91.00  -57.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.1263 -178.0000 -150.0000 34

  2 omega  -95.00  -59.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -36.1263  141.0000  -47.0000 36

  3 omega   17.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1263   38.0000   60.0000 88

  4 omega   17.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1263   38.0000  150.0000 88

  5 omega   37.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1263  178.0000    0.0000 53

  6 omega    9.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       36.1263 -141.0000 -104.0000 88

  7 omega   43.00   77.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000 -180.0000 34

  8 omega   41.00   68.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000   90.0000 27

  9 omega   37.00   69.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000 -150.0000 32

 10 omega   44.00   77.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000    0.0000 33

 11 omega   89.00  161.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000   61.0000   90.0000 72

 12 omega   42.00   69.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000   60.0000 27

 13 omega   47.00   76.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000  -30.0000 29

 14 omega   39.00   64.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000  120.0000 25

 15 omega   44.00  176.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000    0.0000 -120.0000 132

 16 omega   46.00  141.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -91.0000   -1.6527 95

 17 omega   37.00   66.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -30.0000  -60.0000 29

 18 omega   46.00   84.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -95.0000  150.0000 38

 19 omega   40.00   76.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000  -90.0000 36

 20 omega   45.00   71.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -45.0000  150.0000 26

 21 omega   61.00  143.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0000  -93.0000 -177.9648 82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.1804357000
_diffrn_orient_matrix_UB_12      -0.0006519000
_diffrn_orient_matrix_UB_13      -0.0268484000
_diffrn_orient_matrix_UB_21      0.0440376000
_diffrn_orient_matrix_UB_22      -0.0498647000
_diffrn_orient_matrix_UB_23      0.1103294000
_diffrn_orient_matrix_UB_31      0.0392640000
_diffrn_orient_matrix_UB_32      -0.1158822000
_diffrn_orient_matrix_UB_33      -0.0057851000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.1083
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8033
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.113
_diffrn_reflns_theta_min         3.262
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.994
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84614
_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            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       needle
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.142
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         5535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0507P)^2^+2.1636P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1665
_refine_ls_wR_factor_ref         0.1845
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3646
_reflns_number_total             5535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02208h2.cif
_cod_data_source_block           cubr545
_cod_depositor_comments
'Adding full bibliography for 7224588--7224592.cif.'
_cod_database_code               7224592
_chemical_oxdiff_formula         'C58 H48 N6 O2 P2 S2 Br2 Cu2'
_reflns_odcompleteness_completeness 98.13
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.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)
2.b Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'