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_4342428
_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_absolute_configuration ad
_chemical_formula_moiety         'C21 H16 N4 S2'
_chemical_formula_sum            'C21 H16 N4 S2'
_chemical_formula_weight         388.50
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.6062(1)
_cell_length_b                   13.0710(3)
_cell_length_c                   25.3361(5)
_cell_measurement_temperature    133(2)
_cell_volume                     1856.59(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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            12793
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    0.300
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.395
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
'Flack H D (1983),764 Friedel pairs, Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         4219
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0490P)^2^+0.9217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                4010
_reflns_number_total             4219
_reflns_threshold_expression     >2sigma(I)
_publcif_datablock.id            {41cd16e8-7fd5-4d04-b29d-46d3d56d77aa}
_cod_data_source_file            ic5b00064_si_001.cif
_cod_data_source_block           FO5492
_cod_database_code               4342428