Templated Synthesis of the Novel Layered Silver-Antimony Sulfides [H3NCH2CH2NH2][Ag2SbS3] and [H3NCH2CH2NH2]2[Ag5Sb3S8]
Paz Vaqueiro; Ann M. Chippindale; Andrew R. Cowley; Anthony V. Powell; Inorganic Chemistry 42 (2003) 7846–7851; doi:10.1021/ic034926u

data_4312632
_publ_section_title
;
 Templated Synthesis of the Novel Layered Silver-Antimony Sulfides
 [H3NCH2CH2NH2][Ag2SbS3] and [H3NCH2CH2NH2]2[Ag5Sb3S8]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7846
_journal_page_last               7851
_journal_paper_doi               10.1021/ic034926u
_journal_volume                  42
_journal_year                    2003
_chemical_absolute_configuration unk
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C2 H9 Ag2 N2 S3 Sb1 '
_chemical_formula_sum            'C2 H9 Ag2 N2 S3 Sb'
_chemical_formula_weight         494.82
_chemical_melting_point          ?
_chemical_name_systematic
;
?
;
_space_group_IT_number           7
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 111.1637(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   6.1781(1)
_cell_length_b                   11.9491(3)
_cell_length_c                   6.9239(2)
_cell_measurement_reflns_used    1703
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     476.67(2)
_computing_cell_refinement
;
  Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
  COLLECT (Nonius BV, 1997)
;
_computing_data_reduction
;
  Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_computing_molecular_graphics
;
  CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
  CRYSTALS (Watkin et al 2001)
;
_computing_structure_refinement
;
  CRYSTALS (Watkin et al 2001)
;
_computing_structure_solution
;
SIR92
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.938
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type
;
Enraf Nonius Kappa CCD
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6352
_diffrn_reflns_theta_full        22.870
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_min         5.106
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.470
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.13
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' yellow '
_exptl_crystal_density_diffrn    3.447
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' plate '
_exptl_crystal_F_000             456.000
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.23
_refine_diff_density_min         -3.13
_refine_ls_abs_structure_details Flack
_refine_ls_abs_structure_Flack   0.43(4)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9710
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1908
_refine_ls_R_factor_gt           0.0358
_refine_ls_shift/su_max          0.001027
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method = Prince modified Chebychev polynomial, (Watkin, 1994)
  W = [weight] * [1-(deltaF/6*sigmaF)^2]^2
 
  2.99 1.56 1.30
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0372
_refine_ls_wR_factor_ref         0.0372
_reflns_limit_h_max              8
_reflns_limit_h_min              -7
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              -8
_reflns_number_gt                1908
_reflns_number_total             1940
_reflns_threshold_expression     >3.00\s(I)
_cod_data_source_file            ic034926usi20030805_011501_1.cif
_cod_data_source_block           CRYSTALS_cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic ' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 1 n 1 '
_cod_original_formula_sum        ' C2 H9 Ag2 N2 S3 Sb1 '
_cod_database_code               4312632
_refine_ls_r_factor_ref          0.0358