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_7224590
_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_systematic        'CuCl 556'
_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             2015-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2015-10-23 deposited with the CCDC.
2016-03-11 downloaded from the CCDC.
;
_cell_angle_alpha                98.280(3)
_cell_angle_beta                 90.093(2)
_cell_angle_gamma                94.468(2)
_cell_formula_units_Z            1
_cell_length_a                   8.6008(2)
_cell_length_b                   11.9216(4)
_cell_length_c                   13.5031(4)
_cell_measurement_reflns_used    11163
_cell_measurement_temperature    173.0
_cell_measurement_theta_max      71.3310
_cell_measurement_theta_min      4.6310
_cell_volume                     1365.83(7)
_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 0.998
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_details
;
  1 omega  -25.00   42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000 -180.0000 67

  2 omega   32.00   77.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  150.0000 45

  3 omega  -70.00   30.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  -90.0000 100

  4 omega -112.00  -18.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  125.0000  -60.0000 94

  5 omega -128.00  -11.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -19.0000  120.0000 117

  6 omega -112.00  -18.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  125.0000  120.0000 94

  7 omega   33.00  124.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   57.0000   60.0000 91

  8 omega  -14.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -57.0000   90.0000 89

  9 omega   73.00  126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000  120.0000 53

 10 omega   73.00  126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000   60.0000 53

 11 omega  -14.00   75.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -57.0000 -150.0000 89

 12 omega   37.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000  120.0000 53

 13 omega   38.00  148.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000 -180.0000 110

 14 omega   37.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  150.0000 34

 15 omega   37.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -90.0000 35

 16 omega   38.00  148.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000  -90.0000 110

 17 omega   37.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  -60.0000 34

 18 omega   39.00   83.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -50.0000    0.0000 44

 19 omega   79.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000    0.0000 99

 20 omega   37.00   90.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000 -111.0000   60.0000 53

 21 omega   37.00   71.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  120.0000 34

 22 omega   38.00  148.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000   30.0000 110

 23 omega   75.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   25.0000 -180.0000 103

 24 omega   37.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  -30.0000 35

 25 omega   38.00  148.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000  120.0000 110

 26 omega   38.00  148.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000 -150.0000 110

 27 omega   79.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   77.0000  -90.0000 99

 28 omega   38.00  148.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000    0.0000 110

 29 omega   37.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   30.0000 35

 30 omega   37.00   72.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -120.0000 35

 31 omega   79.00  178.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  111.0000   30.0000 99

 32 omega  -44.00   73.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   19.0000 -150.0000 117

 33 omega  -30.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -120.0000 100

 34 omega  -25.00   42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   60.0000 67

 35 omega -125.00  -25.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000  120.0000 100

 36 omega -125.00  -25.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000 -180.0000 100

 37 omega -125.00  -25.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -77.0000   60.0000 100

 38 omega -124.00  -33.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000  -90.0000 91

 39 omega   25.00  125.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000 -150.0000 100

 40 omega   25.00  100.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000 -120.0000 75

 41 omega   73.00  126.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000 -180.0000 53

 42 omega   33.00  124.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   57.0000    0.0000 91

 43 omega   25.00  125.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000  -60.0000 100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0747880000
_diffrn_orient_matrix_UB_12      0.0568995000
_diffrn_orient_matrix_UB_13      -0.0856936000
_diffrn_orient_matrix_UB_21      0.1307644000
_diffrn_orient_matrix_UB_22      -0.0819271000
_diffrn_orient_matrix_UB_23      -0.0065001000
_diffrn_orient_matrix_UB_31      -0.0979391000
_diffrn_orient_matrix_UB_32      -0.0849110000
_diffrn_orient_matrix_UB_33      -0.0768683000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20121
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.589
_diffrn_reflns_theta_min         3.308
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60537
_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 yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0279
_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^)+(0.0390P)^2^+0.4929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4701
_reflns_number_total             5261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce02208h2.cif
_cod_data_source_block           cucl556
_cod_depositor_comments
'Adding full bibliography for 7224588--7224592.cif.'
_cod_database_code               7224590
_chemical_oxdiff_formula         'C58 H48 N6 O2 P2 S2 Cl2 Cu2'
_reflns_odcompleteness_completeness 99.88
_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
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C1(H1), C2(H2), C3(H3A), 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'