Synthesis and Crystal Structures of Ca4SiN4 and New Polymorph of Ca5Si2N6
Hisanori Yamane; Haruhiko Morito; Inorganic Chemistry 52 (2013) 5559–5563; doi:10.1021/ic400522z

data_4334786
_publ_contact_author
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Prof. Dr. Hisanori Yamane
Institute of Multidisciplinary Research for Advanced Materials
Tohoku University
2-1-1 Katahira, Aoba-ku, Sendai
980-8577, Japan
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_publ_contact_author_email       yamane@tagen.tohoku.ac.jp
_publ_contact_author_fax         +81/22/217-5813
_publ_contact_author_phone       +81/22/217-5813
_publ_section_title
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 Synthesis and Crystal Structures of Ca4SiN4 and New Polymorph of Ca5Si2N6
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5559
_journal_page_last               5563
_journal_paper_doi               10.1021/ic400522z
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'N6 Si2, (Ca5)'
_chemical_formula_structural     'Ca5 (Si2N6)'
_chemical_formula_sum            'Ca5 N6 Si2'
_chemical_formula_weight         340.64
_chemical_name_common
; 
calcium silicon nitride
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_chemical_name_systematic
; 
pentacalcium monosilicon hexanitrogen 
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_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.303(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.2712(5)
_cell_length_b                   10.0175(8)
_cell_length_c                   12.0287(8)
_cell_measurement_reflns_used    2919
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.435
_cell_volume                     745.72(10)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku/MSC, 2005)'
_computing_data_collection       'PROCESS-AUTO (Rigaku/MSC, 2005)'
_computing_data_reduction        'PROCESS-AUTO (Rigaku/MSC, 2005)'
_computing_molecular_graphics    'VESTA (Momma & Izumi, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (?)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID II'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0426
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3630
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.87
_exptl_absorpt_coefficient_mu    3.855
_exptl_absorpt_correction_T_max  0.917710
_exptl_absorpt_correction_T_min  0.782615
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
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(NUMABS; Higashi, 1999)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.034
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.092
_exptl_crystal_size_mid          0.067
_exptl_crystal_size_min          0.025
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_matrix_type           full
_refine_ls_number_parameters     68
_refine_ls_number_reflns         895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+14.0090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                759
_reflns_number_total             895
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400522z_si_003_2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
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The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
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_cod_database_code               4334786