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_4322565
_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            'C48 H50 Mg O5 S2'
_chemical_formula_weight         795.3
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                87.3320(10)
_cell_angle_beta                 85.9290(10)
_cell_angle_gamma                68.7330(10)
_cell_formula_units_Z            1
_cell_length_a                   8.4785(4)
_cell_length_b                   9.3595(5)
_cell_length_c                   13.8306(6)
_cell_measurement_reflns_used    3354
_cell_measurement_temperature    150(2)
_cell_volume                     1019.94(9)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_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       \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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6208
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.48
_diffrn_standards_decay_%        No
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.96
_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    1.295
_exptl_crystal_description       block
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.092
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         4475
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.070
_refine_ls_restrained_S_obs      1.138
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_obs          0.0743
_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^)+(0.0521P)^2^+1.9968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1777
_refine_ls_wR_factor_obs         0.1621
_reflns_number_observed          3380
_reflns_number_total             4475
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990814k_1.cif
_cod_data_source_block           Compound_1
_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^)+(0.0521P)^2^+1.9968P] 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^)+(0.0521P)^2^+1.9968P] 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               4322565