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_7046603
_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_formula_moiety         'C28 H54 Cu2 F6 O4 Se3'
_chemical_formula_sum            'C28 H54 Cu2 F6 O4 Se3'
_chemical_formula_weight         932.69
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                91.486(4)
_cell_angle_beta                 92.316(4)
_cell_angle_gamma                104.996(5)
_cell_formula_units_Z            4
_cell_length_a                   12.0827(6)
_cell_length_b                   16.2379(9)
_cell_length_c                   20.2592(10)
_cell_measurement_reflns_used    17891
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      29.5500
_cell_measurement_theta_min      3.8980
_cell_volume                     3833.6(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4685
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.056
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            69037
_diffrn_reflns_theta_full        26.773
_diffrn_reflns_theta_max         30.003
_diffrn_reflns_theta_min         2.904
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.016
_exptl_absorpt_correction_T_max  0.612
_exptl_absorpt_correction_T_min  0.341
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1872
_exptl_crystal_size_max          0.354
_exptl_crystal_size_mid          0.279
_exptl_crystal_size_min          0.155
_refine_diff_density_max         2.38
_refine_diff_density_min         -1.89
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0148
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     775
_refine_ls_number_reflns         19600
_refine_ls_number_restraints     63
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0715
_refine_ls_shift/su_max          0.0028230
_refine_ls_shift/su_mean         0.0001005
_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: 
 0.319E+04 0.399E+04 0.246E+04 839. 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1501
_refine_ls_wR_factor_gt          0.1377
_refine_ls_wR_factor_ref         0.1501
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              22
_reflns_limit_k_min              -21
_reflns_limit_l_max              28
_reflns_limit_l_min              0
_reflns_number_gt                14549
_reflns_number_total             19642
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.33
_oxford_diffrn_Wilson_scale      0.14
_oxford_refine_ls_r_factor_ref   0.0969
_oxford_refine_ls_scale          2.822(15)
_oxford_reflns_number_all        19600
_cod_data_source_file            c8dt01625a2.cif
_cod_data_source_block           I_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7046602--7046603.cif.'
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               7046603
_oxdiff_exptl_absorpt_empirical_full_min 0.695
_oxdiff_exptl_absorpt_empirical_full_max 1.596
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxford_refine_reflns_threshold_expression_ref I>-10.0\s(I)