Ca11E3C8 (E = Sn, Pb): New Complex Carbide Zintl Phases Grown from Ca/Li Flux
Trevor V. Blankenship; Adrian Lita; Susan E. Latturner; Inorganic Chemistry 51 (2012) 13345–13350; doi:10.1021/ic3020833

data_4331338
_publ_contact_author_address
;
 Department of Chemistry and Biochemistry
 Florida State University
 Tallahassee, FL  32306
;
_publ_contact_author_email       latturne@chem.fsu.edu
_publ_contact_author_fax         8506448281
_publ_contact_author_name        'Prof. Susan E. Latturner'
_publ_contact_author_phone       8506444047
_publ_section_title
;
 Ca11E3C8 (E = Sn, Pb): New Complex Carbide Zintl Phases Grown from Ca/Li
 Flux
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              13345
_journal_page_last               13350
_journal_paper_doi               10.1021/ic3020833
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C8 Ca11 Pb3'
_chemical_formula_weight         1158.53
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.6500(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2117(8)
_cell_length_b                   10.7029(7)
_cell_length_c                   14.2493(9)
_cell_measurement_temperature    296(2)
_cell_volume                     1940.2(2)
_computing_cell_refinement       'Saint (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_data_reduction        'Saint (Bruker, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.943
_diffrn_measured_fraction_theta_max 0.943
_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  0.0410
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            21364
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    28.859
_exptl_absorpt_correction_T_max  0.056
_exptl_absorpt_correction_T_min  0.001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    3.966
_exptl_crystal_description       spheroid
_exptl_crystal_F_000             2056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.524
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.244
_refine_ls_extinction_coef       0.000490(19)
_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   1.084
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         4536
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0163P)^2^+10.4769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0576
_reflns_number_gt                4023
_reflns_number_total             4536
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3020833_si_002_1.cif
_cod_data_source_block           ca11pb3c8
_cod_database_code               4331338