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_4343196
_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_formula_moiety         'C12 H10 Cu O4 Se2, C2 H10 Cl2 Cu O3'
_chemical_formula_sum            'C14 H20 Cl2 Cu2 O7 Se2'
_chemical_formula_weight         656.20
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 93.530(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.2186(16)
_cell_length_b                   5.3982(4)
_cell_length_c                   16.8604(12)
_cell_measurement_temperature    293(2)
_cell_volume                     2018.4(3)
_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      373.3
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21173
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.54
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.012
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.669
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear bluish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.159
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         7.146
_refine_diff_density_min         -0.876
_refine_diff_density_rms         0.274
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4558
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1235P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1670
_reflns_number_gt                3717
_reflns_number_total             4558
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00322_si_003.cif
_cod_data_source_block           shelx
_cod_database_code               4343196
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O5-H5
 0.85 with sigma of 0.01
 O6-H6
 0.85 with sigma of 0.01
 C1-H5
 1.909627 with sigma of 0.02
 Cu2-H5
 2.518554 with sigma of 0.02
 C4-H6
 1.913705 with sigma of 0.02
 Cu2-H6
 2.950147 with sigma of 0.02
3. Others
 Sof(C19)=Sof(H19)=Sof(C22)=Sof(H22)=Sof(H24)=Sof(C43)=Sof(H43)=Sof(C48)=
 Sof(H48)=1-FVAR(1)
 Sof(C17)=Sof(H17)=Sof(C21)=Sof(H21)=Sof(H24A)=Sof(C30)=Sof(H30)=Sof(C66)=
 Sof(H66)=FVAR(1)
4.a Rotating group:
 O7(H7A,H7B)
4.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24A), C24(H24),
 C30(H30), C31(H31), C39(H39), C43(H43), C48(H48), C54(H54), C59(H59), C66(H66)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_olex2_submission_special_instructions 'No special instructions were received'