Concept for Enhancement of the Stability of Calcium-Bound Pyrazolyl-Substituted Methanides
Müller, Christoph; Krieck, Sven; Görls, Helmar; Westerhausen, Matthias; Inorganic Chemistry  (2015) 150219085646005–; doi:10.1021/acs.inorgchem.5b00064

data_4342429
_publ_section_title
;
 Concept for Enhancement of the Stability of Calcium-Bound
 Pyrazolyl-Substituted Methanides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              150219085646005
_journal_paper_doi               10.1021/acs.inorgchem.5b00064
_journal_year                    2015
_chemical_formula_moiety         'C31 H43 Ca N5 O2 S2 Si2'
_chemical_formula_sum            'C31 H43 Ca N5 O2 S2 Si2'
_chemical_formula_weight         678.08
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90
_cell_angle_beta                 95.778(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6273(1)
_cell_length_b                   18.4106(2)
_cell_length_c                   18.7911(2)
_cell_measurement_temperature    133(2)
_cell_volume                     3657.89(7)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0279
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29013
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.385
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7133
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.052
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         8377
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0351
_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^)+(0.0275P)^2^+3.0818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0844
_reflns_number_gt                7481
_reflns_number_total             8377
_reflns_threshold_expression     >2sigma(I)
_publcif_datablock.id            {6811659a-4ee1-446d-a2a1-e8323d18c1cb}
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_cod_data_source_file            ic5b00064_si_001.cif
_cod_data_source_block           FO5455
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4342429