Ammonothermal Crystal Growth of Sulfide Materials
Purdy, Andrew P.; Chemistry of Materials 10 (1998) 692–; doi:10.1021/cm970674h

data_4001657
_publ_section_title
;
 Ammonothermal Crystal Growth of Sulfide Materials
;
_journal_issue                   3
_journal_name_full               'Chemistry of Materials'
_journal_page_first              692
_journal_paper_doi               10.1021/cm970674h
_journal_volume                  10
_journal_year                    1998
_chemical_compound_source        'CaS + CuI + NH4I in NH3 at 365 C'
_chemical_formula_analytical     'not determined'
_chemical_formula_moiety         '(NH4 +) (Cu4S3 -)'
_chemical_formula_sum            'Cu4 H4 N S3'
_chemical_formula_weight         368.38
_chemical_melting_point          ?
_chemical_name_common            'Ammonium tetracoppertrisulfide'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           123
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4 2'
_symmetry_space_group_name_H-M   'P 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   3.91010(10)
_cell_length_b                   3.91010(10)
_cell_length_c                   9.4758(6)
_cell_measurement_reflns_used    47
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17.32
_cell_measurement_theta_min      4.3
_cell_volume                     144.874(11)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    'SHELXL-94 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-94 (sheldrick, 1994)'
_computing_structure_refinement  'SHELXL-94 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            680
_diffrn_reflns_theta_max         34.98
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        1.89
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    15.419
_exptl_absorpt_correction_T_max  0.72
_exptl_absorpt_correction_T_min  0.18
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    4.222
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             175
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.354
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.190
_refine_ls_extinction_coef       0.1146(90)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.072
_refine_ls_goodness_of_fit_obs   1.091
_refine_ls_matrix_type           full
_refine_ls_number_parameters     17
_refine_ls_number_reflns         239
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_restrained_S_obs      1.091
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_obs          0.0274
_refine_ls_shift/esd_max         -0.021
_refine_ls_shift/esd_mean        0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.7195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0701
_refine_ls_wR_factor_obs         0.0661
_reflns_number_observed          207
_reflns_number_total             239
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            cm970674h.cif
_cod_data_source_block           pur66t
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_exptl_absorpt_correction_type' value 'Integration' changed
to 'integration' according to
/home/saulius/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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.7195P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0226P)^2^+0.7195P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P4/mmm
_cod_original_formula_sum        'H4 Cu4 N S3'
_cod_database_code               4001657