Syntheses and Structure Determinations of Calcium Thiolates
Scott Chadwick; Ulrich Englich; Bruce Noll; Karin Ruhlandt-Senge; Inorganic Chemistry 37 (1998) 4718–4725; doi:10.1021/ic980086l

data_4322989
_publ_section_title
;
 Syntheses and Structure Determinations of Calcium Thiolates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4718
_journal_page_last               4725
_journal_paper_doi               10.1021/ic980086l
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C11 H9 F5 N2 S'
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_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.261(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.1230(4)
_cell_length_b                   28.543(2)
_cell_length_c                   7.2894(5)
_cell_measurement_reflns_used    2608
_cell_measurement_temperature    150(1)
_cell_volume                     1270.44(15)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    SHELXTL-Plus
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measurement_device       'Siemens SMART CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
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_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
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_diffrn_reflns_theta_min         1.43
_diffrn_standards_decay_%        No
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_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.793
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       needle
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.266
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.183
_refine_ls_hydrogen_treatment    riding
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_refine_ls_number_reflns         2981
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_refine_ls_restrained_S_obs      1.183
_refine_ls_R_factor_all          0.1186
_refine_ls_R_factor_obs          0.0628
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.3566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1215
_refine_ls_wR_factor_obs         0.0986
_reflns_number_observed          1857
_reflns_number_total             2982
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980086l_5.cif
_cod_data_source_block           Compound_5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.3566P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0366P)^2^+0.3566P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2020-11-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_cell_volume        1270.45(14)
_cod_original_formula_sum        'C22 H18 F10 N4 S2'
_cod_original_formula_units_Z    2
_cod_original_formula_weight     592.52
_cod_database_code               4322989