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_4342073
_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         'C40 H52 Ca2 N12 S4'
_chemical_formula_sum            'C40 H52 Ca2 N12 S4'
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_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4771(2)
_cell_length_b                   14.7875(3)
_cell_length_c                   16.0053(3)
_cell_measurement_temperature    133(2)
_cell_volume                     2237.20(8)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0197
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
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_diffrn_reflns_limit_k_min       -19
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_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.486
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.064
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         5093
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_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0350P)^2^+1.4025P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0761
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                4755
_reflns_number_total             5093
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5025907_si_002.cif
_cod_data_source_block           FO5402
_cod_depositor_comments
'Adding full bibliography for 4342066--4342075.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4342073