Ca6[Cr2N6]H, the First Quaternary Nitride-Hydride
Mark S. Bailey; Mark N. Obrovac; Emilie Baillet; Thomas K. Reynolds; David B. Zax; Francis J. DiSalvo; Inorganic Chemistry 42 (2003) 5572–5578; doi:10.1021/ic0343206

data_4314180
_publ_contact_author
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F. J. DiSalvo
102B Baker Laboratory
Dept. of Chemistry and Chemical Biology
Cornell University
Ithaca NY 14853
USA
;
_publ_contact_author_email       fjd3@cornell.edu
_publ_section_title
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 Ca6[Cr2N6]H, the First Quaternary Nitride-Hydride
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5572
_journal_page_last               5578
_journal_paper_doi               10.1021/ic0343206
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'Ca6 Cr2 H2 N6'
_chemical_formula_weight         429.54
_chemical_name_systematic
;
  ?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                   9.0042(2)
_cell_length_b                   9.0042(2)
_cell_length_c                   9.1898(3)
_cell_measurement_temperature    173(2)
_cell_volume                     645.25(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      433(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3591
_diffrn_reflns_theta_full        41.03
_diffrn_reflns_theta_max         41.03
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    6.053
_exptl_absorpt_correction_T_max  0.5828
_exptl_absorpt_correction_T_min  0.3773
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.928
_refine_diff_density_min         -1.014
_refine_diff_density_rms         0.205
_refine_ls_extinction_coef       0.0171(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     24
_refine_ls_number_reflns         884
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^+1.5039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0822
_reflns_number_gt                814
_reflns_number_total             884
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0343206si20030407_111010.cif
_cod_data_source_block           Ca6Cr2N6H
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'H2 Ca6 Cr2 N6'
_cod_database_code               4314180