Reactivity Studies of [(thf)2Mg{μ-C(CH3)2C2H4C(CH3)2}]2: Scrambling Reactions and Diverse Reactions with Dichlorophenylphosphane
Fischer, Reinald; Görls, Helmar; Westerhausen, Matthias; Organometallics 35 (2016) 3861–; doi:10.1021/acs.organomet.6b00743

data_4086802
_publ_section_title
;
 Reactivity Studies of [(thf)2Mg{\m-C(CH3)2C2H4C(CH3)2}]2: Scrambling
 Reactions and Diverse Reactions with Dichlorophenylphosphane
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              3861
_journal_paper_doi               10.1021/acs.organomet.6b00743
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C20 H26 P2 S2'
_chemical_formula_sum            'C20 H26 P2 S2'
_chemical_formula_weight         392.47
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 114.488(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4073(3)
_cell_length_b                   8.0918(2)
_cell_length_c                   16.7052(3)
_cell_measurement_reflns_used    15150
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.73
_cell_volume                     2018.36(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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15150
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         2.73
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7053
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker-AXS, 2002'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.090
_refine_diff_density_max         1.165
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         4601
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0373P)^2^+3.2134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1063
_refine_ls_wR_factor_ref         0.1092
_reflns_number_gt                4230
_reflns_number_total             4601
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om6b00743_si_001.cif
_cod_data_source_block           FO5770
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4086802