Synthesis and structure of [(Ph3P)2Cu(μ-SeCH2Ph)2In(SeCH2Ph)2] as a single-source precursor for the preparation of CuInSe2 nano-materials
Pal, Manoj K.; Dey, Sandip; Neogy, Suman; Kumar, Mukesh; RSC Advances 9 (2019) 18302–; doi:10.1039/C9RA03429C

data_7232886
_publ_section_title
;
 Synthesis and structure of [(Ph3P)2Cu(\m-SeCH2Ph)2In(SeCH2Ph)2] as a
 single-source precursor for the preparation of CuInSe2 nano-materials
;
_journal_issue                   32
_journal_name_full               'RSC Advances'
_journal_page_first              18302
_journal_paper_doi               10.1039/C9RA03429C
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C64 H58 Cu In P2 Se4'
_chemical_formula_sum            'C64 H58 Cu In P2 Se4'
_chemical_formula_weight         1383.24
_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
_audit_creation_date             2017-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2019-04-22 deposited with the CCDC.    2019-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.171(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6988(9)
_cell_length_b                   13.1304(4)
_cell_length_c                   21.1832(10)
_cell_measurement_reflns_used    5803
_cell_measurement_temperature    293
_cell_measurement_theta_max      66.9930
_cell_measurement_theta_min      3.9380
_cell_volume                     5926.3(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3200
_diffrn_detector_type            Titan
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     18.00 112.00   1.00    2.00    --   43.54  57.00 -90.00   94
  2  \w    131.00 157.00   1.00   10.00    --  102.90  77.00-180.00   26
  3  \w     81.00 109.00   1.00   10.00    --  102.90  77.00-180.00   28
  4  \w     36.00 129.00   1.00   10.00    --  102.90 -30.00-180.00   93
  5  \w     52.00 110.00   1.00   10.00    --  102.90 -95.00 -90.00   58
  6  \w     44.00  94.00   1.00   10.00    --  102.90 -77.00 -60.00   50
  7  \w     34.00 142.00   1.00   10.00    --  102.90 -15.00   0.00  108
  8  \w     96.00 157.00   1.00   10.00    --  102.90  15.00  30.00   61
  9  \w     79.00 120.00   1.00   10.00    --  102.90  45.00   0.00   41
 10  \w     72.00  97.00   1.00    2.00    --   43.54 126.00 150.00   25
 11  \w    -26.00  69.00   1.00    2.00    --   43.54 -57.00 120.00   95
 12  \w      9.00  85.00   1.00    2.00    --   43.54-126.00  60.00   76
 13  \w     33.00 122.00   1.00   10.00    --  102.90 -61.00  30.00   89
 14  \w     86.00 121.00   1.00   10.00    --  102.90-126.00 150.00   35
 15  \w     34.00  98.00   1.00   10.00    --  102.90 -95.00  30.00   64
 16  \w     20.00  64.00   1.00   10.00    --  102.90 -95.00-120.00   44
 17  \w     24.00 107.00   1.00   10.00    --  102.90 -95.00-180.00   83
 18  \w   -116.00 -91.00   1.00    2.00    --  -43.54 -99.00 -90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0428068000
_diffrn_orient_matrix_UB_12      0.0891345000
_diffrn_orient_matrix_UB_13      0.0352827000
_diffrn_orient_matrix_UB_21      0.0338214000
_diffrn_orient_matrix_UB_22      -0.0697461000
_diffrn_orient_matrix_UB_23      0.0600461000
_diffrn_orient_matrix_UB_31      0.0474580000
_diffrn_orient_matrix_UB_32      -0.0307559000
_diffrn_orient_matrix_UB_33      -0.0339774000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1022
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17451
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.427
_diffrn_reflns_theta_max         67.427
_diffrn_reflns_theta_min         3.955
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.156
_exptl_absorpt_correction_T_max  0.566
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_description       block
_exptl_crystal_F_000             2744
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.108
_refine_diff_density_max         1.017
_refine_diff_density_min         -1.248
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.1175
_refine_ls_R_factor_gt           0.0684
_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^)+(0.1094P)^2^+15.4635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1727
_refine_ls_wR_factor_ref         0.2523
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3200
_reflns_number_total             5291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra03429c2.cif
_cod_data_source_block           exp_129
_cod_database_code               7232886
_chemical_oxdiff_formula         'C64 Cu In P2 Se4'
_reflns_odcompleteness_completeness 99.33
_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 C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14)
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C32(H32), C28(H28), C5(H5), C16(H16), C26(H26), C23(H23), C10(H10),
 C20(H20), C19(H19), C31(H31), C14(H14), C25(H25), C29(H29), C1(H1), C17(H17),
 C18(H18), C30(H30), C4(H4), C24(H24), C2(H2), C12(H12), C11(H11), C13(H13),
 C3(H3)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2017-10-26
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.735
_oxdiff_exptl_absorpt_empirical_full_min 0.333