Crystal structure of bis(3,3-dimethyl-1-phenylbut-1-en-2-yl)(trimethylsilyl)amido-k1 N)zinc(II), Zn(C15H24NSi)2
Wang, Jun-Hong; Tong, Hong-Bo; Wang, Meng-Liang; Yuan, Hai-Yan; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 719–720; doi:10.1515/ncrs-2021-0057

data_8104690
_publ_section_title
;
 Crystal structure of
 bis(3,3-dimethyl-1-phenylbut-1-en-2-yl)(trimethylsilyl)amido-k1
 N)zinc(II), Zn(C15H24NSi)2
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              719
_journal_page_last               720
_journal_paper_doi               10.1515/ncrs-2021-0057
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C30 H48 N2 Si2 Zn'
_chemical_formula_sum            'C30 H48 N2 Si2 Zn'
_chemical_formula_weight         558.25
_chemical_name_systematic
;
Bis(2-<i>tert</i>-butyl-3-phenyl-1-trimethylsilyl-1-azaallyl-\k^2^<i>N</i>,\\
N')Zinc(II)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     SHELXT
_cell_angle_alpha                74.609(4)
_cell_angle_beta                 73.915(4)
_cell_angle_gamma                64.888(4)
_cell_formula_units_Z            1
_cell_length_a                   8.828(3)
_cell_length_b                   9.458(3)
_cell_length_c                   10.786(3)
_cell_measurement_reflns_used    1382
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.101
_cell_measurement_theta_min      2.874
_cell_volume                     772.1(4)
_computing_cell_refinement       'SAINT v6.02A [1]'
_computing_data_collection       'SMART [1]'
_computing_data_reduction        'SAINT v6.02A [1]'
_computing_molecular_graphics    "'SHELXL-2014/7 [3]"
_computing_publication_material  'SHELXL-2014/7 [3]'
_computing_structure_refinement  'SHELXL-2014/7 [3]'
_computing_structure_solution    'SHELXT-2014/7 [2]'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0496
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3179
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.994
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.9630
_exptl_absorpt_correction_T_min  0.763046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.03 [11] was used for absorption correction.
R(int) was 0.0376 before and 0.0239 after correction.
The Ratio of minimum to maximum transmission is 0.7630.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0762P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2158
_reflns_number_total             2659
_cod_data_source_file            suppl_j_ncrs-2021-0057_suppl.cif
_cod_data_source_block           exp_s333
_cod_database_code               8104690
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
2.b Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;