Phase Transitions and Structures at 10, 92 and 293 K in Eight Trigonal Double Salts <i>M</i>^I^[<i>M</i>^III^(NH~3~)~6~](ClO~4~)~2~<i>X</i>~2~
Figgis, B. N.; Sobolev, A. N.; Reynolds, P. A.; Acta Crystallographica Section B 54 (1998) 613–625; doi:10.1107/S0108768198002328

data_2003151
_publ_section_title
;
 Phase Transitions and Structures at 10, 92 and 293 K in Eight Trigonal
 Double Salts
 <i>M</i>^I^[<i>M</i>^III^(NH~3~)~6~](ClO~4~)~2~<i>X</i>~2~
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              613
_journal_page_last               625
_journal_paper_doi               10.1107/S0108768198002328
_journal_volume                  54
_journal_year                    1998
_chemical_formula_iupac          'N H4[Co(N H3)6],2(Cl O4),Cl2'
_chemical_formula_moiety         'N1 H4,Co1 H18 N6,2(Cl1 O4),2Cl'
_chemical_formula_sum            'Cl4 Co H22 N7 O8'
_chemical_formula_weight         448.98
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   7.0250(10)
_cell_length_b                   7.0250(10)
_cell_length_c                   26.988(12)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    92(2)
_cell_measurement_theta_max      20.5
_cell_measurement_theta_min      16.6
_cell_volume                     1153.4(6)
_computing_cell_refinement       'P3/PC (Siemens, 1989)'
_computing_data_collection       'P3/PC (Siemens, 1989)'
_computing_data_reduction        'PROFIT (Streltsov & Zavodnik, 1989)'
_computing_publication_material  'SHELXTL (Sheldrick, 1983)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      92(2)
_diffrn_measured_fraction_theta_full 0.249
_diffrn_measured_fraction_theta_max 0.249
_diffrn_measurement_device_type  'Siemens P3/P4'
_diffrn_measurement_method       \w/2\q
_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  0.0111
_diffrn_reflns_av_sigmaI/netI    0.0089
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       6
_diffrn_reflns_number            1020
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         6.26
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.855
_exptl_absorpt_correction_T_max  0.7000
_exptl_absorpt_correction_T_min  0.6300
_exptl_absorpt_correction_type   gaussian
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             690
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.219
_refine_ls_extinction_coef       0.0026(10)
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 1983)'
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     40
_refine_ls_number_reflns         347
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0187
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0284P)^2^+1.8943P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0533
_reflns_number_gt                345
_reflns_number_total             347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ta0002.cif
_cod_data_source_block           Ia
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Gaussian' changed to 'gaussian'
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_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Gaussian' changed to
'gaussian' 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^)+(0.0284P)^2^+1.8943P] 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^)+(0.0284P)^2^+1.8943P] 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_Hall     '-P 3*'
_cod_original_sg_symbol_H-M      R-3
_cod_original_formula_sum        'Cl4 Co1 H22 N7 O8'
_cod_database_code               2003151