A Stable Bis(methylene)-λ4-selane with a >C=Se=C< bond containing Se(IV)
Sugamata, Koh; Urao, Yukiko; Minoura, Mao; Chemical Communications  (2019) –; doi:10.1039/C9CC04121D

data_7123673
_publ_section_title
;
 A Stable Bis(methylene)-\l4-selane with a &gt;C=Se=C&lt; bond containing
 Se(IV)
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04121D
_journal_year                    2019
_chemical_formula_moiety         'C54H52Br2SeSi4, C4H10O'
_chemical_formula_sum            'C58 H62 Br2 O Se Si4'
_chemical_formula_weight         1126.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2019-05-14 deposited with the CCDC.    2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.4760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.0334(4)
_cell_length_b                   20.0424(6)
_cell_length_c                   22.4788(6)
_cell_measurement_reflns_used    9948
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      2.51
_cell_volume                     5419.6(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49603
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.512
_exptl_absorpt_coefficient_mu    2.295
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             2312
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: Et2O'
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         12402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0247P)^2^+2.3035P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0760
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8779
_reflns_number_total             12402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04121d2.cif
_cod_data_source_block           190510_CSeC_Br2_urao_0m_a
_cod_database_code               7123673
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.894
_shelx_estimated_absorpt_t_max   0.956
_shelx_res_checksum              56427