Formation of Separated versus Contact Ion Triplets in Magnesium Thiolates. Synthesis and Characterization of [Mg(15-crown-5)(SCPh3)2] and [Mg(15-crown-5)(THF)2][S-2,4,6-tBu3C6H2)]2
Scott Chadwick; Ulrich Englich; Karin Ruhlandt-Senge; Inorganic Chemistry 38 (1999) 6289–6293; doi:10.1021/ic990814k

data_4322566
_publ_section_title
;
 Formation of Separated versus Contact Ion Triplets in Magnesium
 Thiolates. Synthesis and Characterization of [Mg(15-crown-5)(SCPh3)2] and
 [Mg(15-crown-5)(THF)2][S-2,4,6-tBu3C6H2)]2
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6289
_journal_page_last               6293
_journal_paper_doi               10.1021/ic990814k
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C54 H94 Mg O7 S2'
_chemical_formula_weight         943.72
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 97.87
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6755(2)
_cell_length_b                   12.8045(6)
_cell_length_c                   32.7127(12)
_cell_measurement_reflns_used    2881
_cell_measurement_temperature    150(2)
_cell_volume                     5674.3(3)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       omega
_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  0.1024
_diffrn_reflns_av_sigmaI/netI    0.1979
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            15928
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.26
_diffrn_standards_decay_%        No
_exptl_absorpt_coefficient_mu    0.151
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.97
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.105
_exptl_crystal_description       plate
_exptl_crystal_F_000             2072
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.357
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.00044(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.000
_refine_ls_goodness_of_fit_obs   1.174
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     573
_refine_ls_number_reflns         9120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_restrained_S_obs      1.174
_refine_ls_R_factor_all          0.2005
_refine_ls_R_factor_obs          0.0909
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1774
_refine_ls_wR_factor_obs         0.1397
_reflns_number_observed          4349
_reflns_number_total             9120
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990814k_2.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.0000P] 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^)+(0.0507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4322566