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

data_4001658
_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         '(Ca 2+) (Cu2S2 2-)'
_chemical_formula_sum            'Ca Cu2 S2'
_chemical_formula_weight         231.28
_chemical_melting_point          ?
_chemical_name_common            'calcium copper sulfide'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           164
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 3 2"'
_symmetry_space_group_name_H-M   'P -3 m 1'
_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                120.00
_cell_formula_units_Z            1
_cell_length_a                   3.9400(4)
_cell_length_b                   3.9400(4)
_cell_length_c                   6.5230(13)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.16
_cell_measurement_theta_min      3.12
_cell_volume                     87.69(2)
_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  0.0488
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            752
_diffrn_reflns_theta_max         44.85
_diffrn_reflns_theta_min         3.12
_diffrn_standards_decay_%        8.38
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    14.498
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.14
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.379
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             110
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.021
_refine_diff_density_min         -2.289
_refine_diff_density_rms         0.325
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.128
_refine_ls_goodness_of_fit_obs   1.153
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     9
_refine_ls_number_reflns         306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_restrained_S_obs      1.153
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_obs          0.0463
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+0.3450P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1390
_refine_ls_wR_factor_obs         0.1283
_reflns_number_observed          251
_reflns_number_total             306
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            cm970674h.cif
_cod_data_source_block           pur68z
_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.

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^)+(0.0658P)^2^+0.3450P] 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^)+(0.0658P)^2^+0.3450P] 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      P-3m
_cod_database_code               4001658