Ionothermal syntheses of nano- and microstructured ternary copper-indium-chalcogenides.
Tyrrell, Sophie; Behrendt, Gereon; Nockemann, Peter; Inorganic chemistry 54 (2015) 4495–4503; doi:10.1021/acs.inorgchem.5b00322

data_4343194
_publ_section_title
;
 Ionothermal syntheses of nano- and microstructured ternary
 copper-indium-chalcogenides.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4495
_journal_page_last               4503
_journal_paper_doi               10.1021/acs.inorgchem.5b00322
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C24 H20 Cl Cu Se4'
_chemical_formula_sum            'C24 H20 Cl Cu Se4'
_chemical_formula_weight         723.23
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-02-03
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.06 svn.r3123 for OlexSys, GUI svn.r4979)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.859(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.5566(10)
_cell_length_b                   5.7532(4)
_cell_length_c                   14.7074(10)
_cell_measurement_temperature    100(2)
_cell_volume                     1146.48(14)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0926
_diffrn_reflns_av_unetI/netI     0.1083
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15312
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.01
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           55.0
_diffrn_source_power             2.475
_diffrn_source_voltage           45.0
_exptl_absorpt_coefficient_mu    7.429
_exptl_absorpt_correction_T_max  0.9294
_exptl_absorpt_correction_T_min  0.6244
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.934
_refine_diff_density_min         -1.017
_refine_diff_density_rms         0.181
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         4953
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+1.1668P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                3864
_reflns_number_total             4953
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00322_si_002.cif
_cod_data_source_block           2012ncs0784a
_cod_database_code               4343194
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C16(H16), C4(H4), C5(H5), C14(H14), C18(H18), C15(H15), C21(H21), C20(H20),
 C3(H3), C6(H6), C23(H23), C24(H24), C2(H2), C17(H17), C22(H22), C12(H12),
 C10(H10), C8(H8), C9(H9), C11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'