Tris(pyrazolyl)methanides of the Alkaline Earth Metals: Influence of the Substitution Pattern on Stability and Degradation.
Müller, Christoph; Koch, Alexander; Görls, Helmar; Krieck, Sven; Westerhausen, Matthias; Inorganic chemistry 54 (2015) 635–645; doi:10.1021/ic5025907

data_4342070
_publ_section_title
;
 Tris(pyrazolyl)methanides of the Alkaline Earth Metals: Influence of the
 Substitution Pattern on Stability and Degradation.
;
_journal_issue                   2
_journal_name_full               'Inorganic chemistry'
_journal_page_first              635
_journal_page_last               645
_journal_paper_doi               10.1021/ic5025907
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C22 H16 N6 S3'
_chemical_formula_sum            'C22 H16 N6 S3'
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_symmetry_cell_setting           monoclinic
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_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9824(2)
_cell_length_b                   21.6608(4)
_cell_length_c                   10.9294(2)
_cell_measurement_temperature    133(2)
_cell_volume                     2102.40(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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0293
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
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_diffrn_reflns_limit_l_min       -14
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_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    0.376
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6650
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.045
_exptl_crystal_size_mid          0.042
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4815
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0282P)^2^+3.4136P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1088
_reflns_number_gt                4194
_reflns_number_total             4815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5025907_si_002.cif
_cod_data_source_block           FO5412
_cod_depositor_comments
'Adding full bibliography for 4342066--4342075.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4342070