LiCa3As2H and Ca14As6X7 (X = C, H, N): Two New Arsenide Hydride Phases Grown from Ca/Li Metal Flux.
Blankenship, Trevor V.; Wang, Xiaoping; Hoffmann, Christina; Latturner, Susan E.; Inorganic chemistry 53 (2014) 10620–10626; doi:10.1021/ic501722d

data_4341481
_publ_section_title
;
 LiCa3As2H and Ca14As6X7 (X = C, H, N): Two New Arsenide Hydride Phases
 Grown from Ca/Li Metal Flux.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10620
_journal_page_last               10626
_journal_paper_doi               10.1021/ic501722d
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C0.445 H4.915 As6 Ca14 N1.135'
_chemical_formula_weight         1036.79
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           127
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4 2ab'
_symmetry_space_group_name_H-M   'P 4/m b m'
_atom_sites_solution_hydrogens   difmap
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7027(2)
_cell_length_b                   15.7027(2)
_cell_length_c                   9.1043(2)
_cell_measurement_temperature    100(2)
_cell_volume                     2244.89(6)
_computing_cell_refinement       Mantid
_computing_data_collection       'SNS PyDas'
_computing_data_reduction        'Mantid and anvred2x'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.709
_diffrn_measured_fraction_theta_max 0.448
_diffrn_measurement_device_type  'TOPAZ 6-Li-glass area detectors at the SNS'
_diffrn_measurement_method       'TOF Laue'
_diffrn_radiation_source         'Spallation Neutron Source at ORNL, USA'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     '0.5 - 3.5'
_diffrn_reflns_av_R_equivalents  0.0858
_diffrn_reflns_av_sigmaI/netI    0.0701
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7364
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         36.31
_diffrn_reflns_theta_min         2.89
_exptl_absorpt_coefficient_mu    0.0700
_exptl_absorpt_correction_T_max  0.9722
_exptl_absorpt_correction_T_min  0.9255
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
The linear absorption coefficient is wavelength dependent
and it is calculated as:
          mu = 0.333 + 0.367 * lambda  [cm^-1^]
The value of 0.07000 (mm^-1^)given in _exptl_absorpt_coefficient_mu
is the value at 1 \%A
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.068
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             402
_exptl_crystal_size_max          1.20
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.70
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.082
_refine_diff_density_rms         0.185
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.180
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1330
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0259P)^2^+8.0088P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                1322
_reflns_number_total             1330
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic501722d_si_002.cif
_cod_data_source_block           Ca14As6X7neutron
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 
;
_cod_original_formula_sum        'Ca14 As6 C0.445 N1.135 H4.915'
_cod_database_code               4341481