Isolation of a 1-Magnesium-2,3-Disilacyclopropene and a Related Bis(disilenide).
Tian, Miao; Zhang, Jianying; Yang, Hao; Cui, Chunming; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00519

data_4134224
_publ_section_title
;
 Isolation of a 1-Magnesium-2,3-Disilacyclopropene and a Related
 Bis(disilenide).
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00519
_journal_year                    2020
_chemical_formula_moiety         'C64 H96 B2 Mg N4 O3 Si2'
_chemical_formula_sum            'C64 H96 B2 Mg N4 O3 Si2'
_chemical_formula_weight         1071.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
????
;
_cell_angle_alpha                90
_cell_angle_beta                 95.29(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.594(3)
_cell_length_b                   22.789(5)
_cell_length_c                   23.453(5)
_cell_measurement_reflns_used    7491
_cell_measurement_temperature    113.15
_cell_measurement_theta_max      27.8784
_cell_measurement_theta_min      1.7441
_cell_volume                     7235(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1271
_diffrn_reflns_av_unetI/netI     0.1018
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57151
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.150
_diffrn_reflns_theta_max         24.150
_diffrn_reflns_theta_min         1.744
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8982
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.984
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.291
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         11553
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1469
_refine_ls_R_factor_gt           0.0829
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1249P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2060
_refine_ls_wR_factor_ref         0.2412
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6514
_reflns_number_total             11553
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00519_si_002.cif
_cod_data_source_block           tm_sq
_cod_database_code               4134224
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.981
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C50(H50), C38(H38), C12(H12), C47(H47), C24(H24), C35(H35), C21(H21), C9(H9)
2.b Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C59(H59A,H59B), C57(H57A,H57B), C56(H56A,H56B), C61(H61A,
 H61B), C58(H58A,H58B), C53(H53A,H53B), C55(H55A,H55B), C62(H62A,H62B),
 C63(H63A,H63B), C64(H64A,H64B), C54(H54A,H54B)
2.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C27(H27), C2(H2), C1(H1), C5(H5), C45(H45), C43(H43), C6(H6),
 C7(H7), C31(H31), C19(H19), C44(H44), C33(H33), C17(H17), C32(H32), C18(H18)
2.d Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C39(H39A,H39B,H39C), C51(H51A,H51B,H51C), C25(H25A,H25B,
 H25C), C14(H14A,H14B,H14C), C40(H40A,H40B,H40C), C48(H48A,H48B,H48C), C11(H11A,
 H11B,H11C), C49(H49A,H49B,H49C), C37(H37A,H37B,H37C), C26(H26A,H26B,H26C),
 C36(H36A,H36B,H36C), C13(H13A,H13B,H13C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              77512
_shelx_hkl_checksum              35634
_shelx_fab_checksum              89270
_olex2_submission_special_instructions 'No special instructions were received'