#------------------------------------------------------------------------------
#$Date: 2015-04-02 14:22:18 +0300 (Thu, 02 Apr 2015) $
#$Revision: 134621 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/16/4001658.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4001658
loop_
_publ_author_name
'Purdy, Andrew P.'
_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)
_[local]_cod_data_source_file    cm970674h.cif
_[local]_cod_data_source_block   pur68z
_[local]_cod_cif_authors_sg_H-M  P-3m
_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_database_code               4001658
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cu1 0.0204(3) 0.0204(3) 0.0184(4) 0.000 0.000 0.0102(2)
Ca1 0.0102(3) 0.0102(3) 0.0107(5) 0.000 0.000 0.0051(2)
S1 0.0093(3) 0.0093(3) 0.0092(4) 0.000 0.000 0.0046(2)
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.3333 0.6667 0.37649(15) 0.0197(3) Uani 1 d S
Ca1 Ca 0.0000 1.0000 1.0000 0.0104(2) Uani 1 d S
S1 S 0.3333 0.6667 0.7463(2) 0.0092(2) Uani 1 d S
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
S1 Cu1 S1 109.55(4) 7_676 7_566
S1 Cu1 S1 109.55(4) 7_676 7_666
S1 Cu1 S1 109.55(4) 7_566 7_666
S1 Cu1 S1 109.39(4) 7_676 .
S1 Cu1 S1 109.39(4) 7_566 .
S1 Cu1 S1 109.39(4) 7_666 .
S1 Cu1 Cu1 54.70(3) 7_676 7_676
S1 Cu1 Cu1 125.22(2) 7_566 7_676
S1 Cu1 Cu1 125.22(2) 7_666 7_676
S1 Cu1 Cu1 54.69(3) . 7_676
S1 Cu1 Cu1 125.22(2) 7_676 7_566
S1 Cu1 Cu1 54.70(3) 7_566 7_566
S1 Cu1 Cu1 125.22(2) 7_666 7_566
S1 Cu1 Cu1 54.69(3) . 7_566
Cu1 Cu1 Cu1 89.93(5) 7_676 7_566
S1 Cu1 Cu1 125.22(2) 7_676 7_666
S1 Cu1 Cu1 125.22(2) 7_566 7_666
S1 Cu1 Cu1 54.70(3) 7_666 7_666
S1 Cu1 Cu1 54.69(3) . 7_666
Cu1 Cu1 Cu1 89.93(5) 7_676 7_666
Cu1 Cu1 Cu1 89.93(5) 7_566 7_666
S1 Cu1 Ca1 55.66(3) 7_676 1_554
S1 Cu1 Ca1 55.66(3) 7_566 1_554
S1 Cu1 Ca1 113.42(5) 7_666 1_554
S1 Cu1 Ca1 137.192(13) . 1_554
Cu1 Cu1 Ca1 98.44(2) 7_676 1_554
Cu1 Cu1 Ca1 98.44(2) 7_566 1_554
Cu1 Cu1 Ca1 168.12(4) 7_666 1_554
S1 Cu1 Ca1 55.66(3) 7_676 1_654
S1 Cu1 Ca1 113.42(5) 7_566 1_654
S1 Cu1 Ca1 55.66(3) 7_666 1_654
S1 Cu1 Ca1 137.192(13) . 1_654
Cu1 Cu1 Ca1 98.44(2) 7_676 1_654
Cu1 Cu1 Ca1 168.12(4) 7_566 1_654
Cu1 Cu1 Ca1 98.44(2) 7_666 1_654
Ca1 Cu1 Ca1 72.10(2) 1_554 1_654
S1 Cu1 Ca1 113.42(5) 7_676 1_544
S1 Cu1 Ca1 55.66(3) 7_566 1_544
S1 Cu1 Ca1 55.66(3) 7_666 1_544
S1 Cu1 Ca1 137.192(13) . 1_544
Cu1 Cu1 Ca1 168.12(4) 7_676 1_544
Cu1 Cu1 Ca1 98.44(2) 7_566 1_544
Cu1 Cu1 Ca1 98.44(2) 7_666 1_544
Ca1 Cu1 Ca1 72.10(2) 1_554 1_544
Ca1 Cu1 Ca1 72.10(2) 1_654 1_544
S1 Ca1 S1 180.0 . 7_577
S1 Ca1 S1 88.90(3) . 1_565
S1 Ca1 S1 91.10(3) 7_577 1_565
S1 Ca1 S1 88.90(3) . 1_455
S1 Ca1 S1 91.10(3) 7_577 1_455
S1 Ca1 S1 88.90(3) 1_565 1_455
S1 Ca1 S1 91.10(3) . 7_677
S1 Ca1 S1 88.90(3) 7_577 7_677
S1 Ca1 S1 91.10(3) 1_565 7_677
S1 Ca1 S1 180.0 1_455 7_677
S1 Ca1 S1 91.10(3) . 7_567
S1 Ca1 S1 88.90(3) 7_577 7_567
S1 Ca1 S1 180.0 1_565 7_567
S1 Ca1 S1 91.10(3) 1_455 7_567
S1 Ca1 S1 88.90(3) 7_677 7_567
S1 Ca1 Cu1 96.77(3) . 7_576
S1 Ca1 Cu1 83.23(3) 7_577 7_576
S1 Ca1 Cu1 45.059(13) 1_565 7_576
S1 Ca1 Cu1 45.059(13) 1_455 7_576
S1 Ca1 Cu1 134.942(13) 7_677 7_576
S1 Ca1 Cu1 134.942(13) 7_567 7_576
S1 Ca1 Cu1 83.23(3) . 1_556
S1 Ca1 Cu1 96.77(3) 7_577 1_556
S1 Ca1 Cu1 134.942(13) 1_565 1_556
S1 Ca1 Cu1 134.941(13) 1_455 1_556
S1 Ca1 Cu1 45.058(13) 7_677 1_556
S1 Ca1 Cu1 45.058(13) 7_567 1_556
Cu1 Ca1 Cu1 180.0 7_576 1_556
S1 Ca1 Cu1 45.059(13) . 7_676
S1 Ca1 Cu1 134.942(13) 7_577 7_676
S1 Ca1 Cu1 45.059(13) 1_565 7_676
S1 Ca1 Cu1 96.77(3) 1_455 7_676
S1 Ca1 Cu1 83.23(3) 7_677 7_676
S1 Ca1 Cu1 134.941(13) 7_567 7_676
Cu1 Ca1 Cu1 72.10(2) 7_576 7_676
Cu1 Ca1 Cu1 107.90(2) 1_556 7_676
S1 Ca1 Cu1 45.059(13) . 7_566
S1 Ca1 Cu1 134.942(13) 7_577 7_566
S1 Ca1 Cu1 96.77(3) 1_565 7_566
S1 Ca1 Cu1 45.059(13) 1_455 7_566
S1 Ca1 Cu1 134.941(13) 7_677 7_566
S1 Ca1 Cu1 83.23(3) 7_567 7_566
Cu1 Ca1 Cu1 72.10(2) 7_576 7_566
Cu1 Ca1 Cu1 107.90(2) 1_556 7_566
Cu1 Ca1 Cu1 72.10(2) 7_676 7_566
S1 Ca1 Cu1 134.941(13) . 1_566
S1 Ca1 Cu1 45.058(13) 7_577 1_566
S1 Ca1 Cu1 83.23(3) 1_565 1_566
S1 Ca1 Cu1 134.941(13) 1_455 1_566
S1 Ca1 Cu1 45.059(13) 7_677 1_566
S1 Ca1 Cu1 96.77(3) 7_567 1_566
Cu1 Ca1 Cu1 107.90(2) 7_576 1_566
Cu1 Ca1 Cu1 72.10(2) 1_556 1_566
Cu1 Ca1 Cu1 107.90(2) 7_676 1_566
Cu1 Ca1 Cu1 180.0 7_566 1_566
S1 Ca1 Cu1 134.941(13) . 1_456
S1 Ca1 Cu1 45.058(13) 7_577 1_456
S1 Ca1 Cu1 134.941(13) 1_565 1_456
S1 Ca1 Cu1 83.23(3) 1_455 1_456
S1 Ca1 Cu1 96.77(3) 7_677 1_456
S1 Ca1 Cu1 45.059(13) 7_567 1_456
Cu1 Ca1 Cu1 107.90(2) 7_576 1_456
Cu1 Ca1 Cu1 72.10(2) 1_556 1_456
Cu1 Ca1 Cu1 180.0 7_676 1_456
Cu1 Ca1 Cu1 107.90(2) 7_566 1_456
Cu1 Ca1 Cu1 72.10(2) 1_566 1_456
Cu1 S1 Cu1 109.55(4) 7_676 7_566
Cu1 S1 Cu1 109.55(4) 7_676 7_666
Cu1 S1 Cu1 109.55(4) 7_566 7_666
Cu1 S1 Cu1 70.61(4) 7_676 .
Cu1 S1 Cu1 70.61(4) 7_566 .
Cu1 S1 Cu1 70.61(4) 7_666 .
Cu1 S1 Ca1 79.28(2) 7_676 .
Cu1 S1 Ca1 79.28(2) 7_566 .
Cu1 S1 Ca1 163.35(6) 7_666 .
Cu1 S1 Ca1 126.04(2) . .
Cu1 S1 Ca1 79.28(2) 7_676 1_655
Cu1 S1 Ca1 163.35(6) 7_566 1_655
Cu1 S1 Ca1 79.28(2) 7_666 1_655
Cu1 S1 Ca1 126.04(2) . 1_655
Ca1 S1 Ca1 88.90(3) . 1_655
Cu1 S1 Ca1 163.35(6) 7_676 1_545
Cu1 S1 Ca1 79.28(2) 7_566 1_545
Cu1 S1 Ca1 79.28(2) 7_666 1_545
Cu1 S1 Ca1 126.04(2) . 1_545
Ca1 S1 Ca1 88.90(3) . 1_545
Ca1 S1 Ca1 88.90(3) 1_655 1_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 S1 2.4115(6) 7_676
Cu1 S1 2.4115(6) 7_566
Cu1 S1 2.4116(6) 7_666
Cu1 S1 2.412(2) .
Cu1 Cu1 2.7877(11) 7_676
Cu1 Cu1 2.7877(11) 7_566
Cu1 Cu1 2.7877(11) 7_666
Cu1 Ca1 3.3475(8) 1_554
Cu1 Ca1 3.3475(8) 1_654
Cu1 Ca1 3.3475(8) 1_544
Ca1 S1 2.8132(8) .
Ca1 S1 2.8132(8) 7_577
Ca1 S1 2.8132(8) 1_565
Ca1 S1 2.8132(8) 1_455
Ca1 S1 2.8132(8) 7_677
Ca1 S1 2.8132(8) 7_567
Ca1 Cu1 3.3474(8) 7_576
Ca1 Cu1 3.3475(8) 1_556
Ca1 Cu1 3.3475(8) 7_676
Ca1 Cu1 3.3475(8) 7_566
Ca1 Cu1 3.3475(8) 1_566
Ca1 Cu1 3.3475(8) 1_456
S1 Cu1 2.4115(6) 7_676
S1 Cu1 2.4115(6) 7_566
S1 Cu1 2.4116(6) 7_666
S1 Ca1 2.8132(8) 1_655
S1 Ca1 2.8132(8) 1_545