Precursor-mediated synthesis of Cu<sub>2-x</sub>Se nanoparticles and their composites with TiO<sub>2</sub> for improved photocatalysis.
Gahlot, Sweta; Jeanneau, Erwann; Dappozze, Frederic; Guillard, Chantal; Mishra, Shashank; Dalton transactions (Cambridge, England : 2003) 47 (2018) 8897–8905; doi:10.1039/c8dt01625a

data_7046602
_publ_section_title
;
 Precursor-mediated synthesis of Cu<sub>2-x</sub>Se nanoparticles and
 their composites with TiO<sub>2</sub> for improved photocatalysis.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8897
_journal_page_last               8905
_journal_paper_doi               10.1039/c8dt01625a
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C32 H72 Cu4 I4 Se4'
_chemical_formula_sum            'C32 H72 Cu4 I4 Se4'
_chemical_formula_weight         1534.56
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_update_record
;
2018-05-27 deposited with the CCDC.
2018-06-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.390(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7484(4)
_cell_length_b                   14.7713(3)
_cell_length_c                   22.8613(7)
_cell_measurement_reflns_used    11832
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      28.4480
_cell_measurement_theta_min      3.8370
_cell_volume                     4939.0(2)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9897
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Nova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            21683
_diffrn_reflns_theta_full        26.609
_diffrn_reflns_theta_max         29.378
_diffrn_reflns_theta_min         3.185
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.167
_exptl_absorpt_correction_T_max  0.949
_exptl_absorpt_correction_T_min  0.397
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (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            colorless
_exptl_crystal_density_diffrn    2.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.236
_exptl_crystal_size_mid          0.149
_exptl_crystal_size_min          0.077
_refine_diff_density_max         4.50
_refine_diff_density_min         -2.74
_refine_ls_abs_structure_details
; 
 Parsons, Flack & Wagner (2013), 
 3746 Friedel Pairs 
;
_refine_ls_abs_structure_Flack   0.132(11)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9738
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         9995
_refine_ls_number_restraints     274
_refine_ls_R_factor_all          0.1167
_refine_ls_R_factor_gt           0.1127
_refine_ls_shift/su_max          0.0022981
_refine_ls_shift/su_mean         0.0000955
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 0.484E+04 0.736E+04 0.327E+04 0.225E+04 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2373
_refine_ls_wR_factor_gt          0.2362
_refine_ls_wR_factor_ref         0.2371
_reflns_limit_h_max              19
_reflns_limit_h_min              -20
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              -30
_reflns_number_gt                9449
_reflns_number_total             10065
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.91
_oxford_diffrn_Wilson_scale      2.58
_oxford_refine_ls_r_factor_ref   0.1163
_oxford_refine_ls_scale          0.980(4)
_oxford_reflns_number_all        10043
_cod_data_source_file            c8dt01625a2.cif
_cod_data_source_block           I
_cod_depositor_comments
;
Adding full bibliography for 7046602--7046603.cif.

2025-03-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'C 1 c 1 '
_cod_original_formula_moiety     'C64 H144 Cu8 I8 Se8'
_cod_original_formula_sum        'C64 H144 Cu8 I8 Se8'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     3069.13
_cod_database_code               7046602
_oxdiff_exptl_absorpt_empirical_full_min 0.859
_oxdiff_exptl_absorpt_empirical_full_max 1.198
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxford_refine_reflns_threshold_expression_ref I>0.0\s(I)
_oxford_hooft_y                  0.125(15)
_oxford_bijvoet_difference       0.132(11)
_oxford_refined_flack_x          0.15(5)