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_4343195
_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         '0.33(Cl10 Cu5 O), C12 H23 N2'
_chemical_formula_sum            'C12 H23 Cl3.33 Cu1.67 N2 O0.33'
_chemical_formula_weight         424.72
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.777(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   19.8719(14)
_cell_length_b                   9.0935(5)
_cell_length_c                   29.202(2)
_cell_measurement_temperature    293(2)
_cell_volume                     5274.4(6)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1301
_diffrn_reflns_av_unetI/netI     0.1329
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            36327
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.52
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.524
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2600
_refine_diff_density_max         2.074
_refine_diff_density_min         -1.166
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     529
_refine_ls_number_reflns         12051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1485
_refine_ls_R_factor_gt           0.0966
_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^)+(0.1455P)^2^+5.7929P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2494
_refine_ls_wR_factor_ref         0.2787
_reflns_number_gt                7262
_reflns_number_total             12051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b00322_si_004.cif
_cod_data_source_block           2014ncs0062a
_cod_database_code               4343195
_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
2.a Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C31(H31A,H31B), C10(H10A,H10B), C23(H23A,H23B), C9(H9A,H9B),
 C29(H29A,H29B), C6(H6A,H6B), C19(H19A,H19B), C8(H8A,H8B), C33(H33A,H33B),
 C5(H5A,H5B), C20(H20A,H20B), C32(H32A,H32B), C22(H22A,H22B), C18(H18A,H18B),
 C21(H21A,H21B), C11(H11A,H11B), C35(H35A,H35B), C34(H34A,H34B), C17(H17A,H17B),
  C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C25(H25), C13(H13), C15(H15), C26(H26), C14(H14), C1(H1), C27(H27), C3(H3),
 C2(H2)
2.c Idealised Me refined as rotating group:
 C36(H36A,H36B,H36C), C28(H28A,H28B,H28C), C4(H4A,H4B,H4C), C24(H24A,H24B,
 H24C), C16(H16A,H16B,H16C), C12(H12A,H12B,H12C)
;
_olex2_computing_structure_refinement_long 'ShelXL (Sheldrick, 2008)'
_olex2_computing_structure_solution_long 'ShelXS (Sheldrick, 2008)'
_olex2_submission_special_instructions 'No special instructions were received'