Synthesis and structure of new mixed alkaline-earth nitridomolybdates and nitridotungstates, (Ba,Ca)3[MN4] (M = Mo, W)
Baker, Charles F.; Barker, Marten G.; Blake, Alexander J.; Wilson, Claire; Gregory, Duncan H.; Dalton Transactions  (2003) 1065–1069; doi:10.1039/b211138a

data_7012467
_publ_section_title
;
 Synthesis and structure of new mixed alkaline-earth nitridomolybdates
 and nitridotungstates, (Ba,Ca)3[MN4] (M = Mo, W)
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1065
_journal_page_last               1069
_journal_paper_doi               10.1039/b211138a
_journal_year                    2003
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'Ba6 Ca6 N16 W4'
_chemical_formula_sum            'Ba1.44 Ca1.56 N4 W'
_chemical_formula_weight         499.94
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2002-10-25T09:52:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.3049(10)
_cell_length_b                   9.5822(9)
_cell_length_c                   11.7405(11)
_cell_measurement_reflns_used    1401
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.56
_cell_measurement_theta_min      3.38
_cell_volume                     1159.30(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'ATOMS 4.1 (Dowty, 1998)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'Bruker Smart CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.047
_diffrn_reflns_av_unetI/netI     0.044
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4876
_diffrn_reflns_theta_full        28.69
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         3.38
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    30.754
_exptl_absorpt_correction_T_max  0.296
_exptl_absorpt_correction_T_min  0.149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SAINT V6.01/SADABS'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    5.729
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1710
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.19
_refine_diff_density_min         -3.204
_refine_diff_density_rms         0.47
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.94
_refine_ls_matrix_type           full
_refine_ls_number_parameters     74
_refine_ls_number_reflns         1352
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                1058
_reflns_number_total             1564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b211138a.txt
_cod_data_source_block           cabawn
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multiscan' changed to
'multi-scan' 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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] 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^)+(0.0474P)^2^+0.0000P] 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      Pbca
_cod_database_code               7012467