A series of dinuclear cuprous iodide complexes chelated with 1,2-bis(diphenylphosphino)benzene derivatives: structural, photophysical and thermal properties
Li, Xiaoyue; Zhang, Juanye; Wei, Feng; Liu, Xiaochen; Liu, Zhiwei; Bian, Zuqiang; Huang, Chunhui; CrystEngComm 18 (2016) 4388–; doi:10.1039/C5CE02533H

data_7224848
_publ_section_title
;
 A series of dinuclear cuprous iodide complexes chelated with
 1,2-bis(diphenylphosphino)benzene derivatives: structural, photophysical
 and thermal properties
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              4388
_journal_paper_doi               10.1039/C5CE02533H
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C64 H56 Cu2 I2 O4 P4, 3(C H2 Cl2)'
_chemical_formula_sum            'C67 H62 Cl6 Cu2 I2 O4 P4'
_chemical_formula_weight         1648.63
_chemical_name_common            '[Cu(\m-I)OMe-dppb]2'
_chemical_name_systematic
'4,5-dimethoxyl-1,2-bis(diphenylphosphino) benzene'
_chemical_properties_physical    'Efflorescent, Oxygen-sensitive'
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-21 deposited with the CCDC.
2016-04-06 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 113.268(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.5414(11)
_cell_length_b                   14.5730(6)
_cell_length_c                   26.9535(14)
_cell_measurement_reflns_used    7075
_cell_measurement_temperature    180.01(10)
_cell_measurement_theta_max      26.6970
_cell_measurement_theta_min      3.1590
_cell_volume                     7051.4(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      180.01(10)
_diffrn_detector_area_resol_mean 10.3914
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -59.00   35.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  -57.0000  150.0000 94

  2 omega  -20.00   53.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017  -99.0000   60.0000 73

  3 omega  -14.00   79.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       10.7017   57.0000  -60.0000 93
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0183027000
_diffrn_orient_matrix_UB_12      -0.0385453000
_diffrn_orient_matrix_UB_13      0.0156905000
_diffrn_orient_matrix_UB_21      0.0347786000
_diffrn_orient_matrix_UB_22      0.0172734000
_diffrn_orient_matrix_UB_23      0.0016147000
_diffrn_orient_matrix_UB_31      0.0043117000
_diffrn_orient_matrix_UB_32      0.0241432000
_diffrn_orient_matrix_UB_33      0.0238922000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0567
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            21359
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         3.17
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.842
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'green '
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prims
_exptl_crystal_F_000             3288
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane /n-pentane '
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.790
_refine_diff_density_rms         0.094
_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     386
_refine_ls_number_reflns         6918
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0392P)^2^+14.2922P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.1039
_reflns_number_gt                5114
_reflns_number_total             6918
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ce02533h2.cif
_cod_data_source_block           exp_6324
_cod_depositor_comments
'Adding full bibliography for 7224847--7224849.cif.'
_cod_original_cell_volume        7051.5(6)
_cod_database_code               7224848
_chemical_oxdiff_formula         'C1 H1 O1 Cu1'
_reflns_odcompleteness_completeness 99.75
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H34A(0.5) H34B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C22(H22), C23(H23), C24(H24), C25(H25),
  C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_olex2_submission_special_instructions 'No special instructions were received'