Synthesis, characterisation, and dehydrocoupling ability of zirconium complexes bearing hindered bis(amido)silyl ligands.
Lummis, Paul A.; McDonald, Robert; Ferguson, Michael J.; Rivard, Eric; Dalton transactions (Cambridge, England : 2003) 44 (2015) 7009–7020; doi:10.1039/c5dt00306g

data_7034308
_publ_section_title
;
 Synthesis, characterisation, and dehydrocoupling ability of zirconium
 complexes bearing hindered bis(amido)silyl ligands.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7009
_journal_page_last               7020
_journal_paper_doi               10.1039/c5dt00306g
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C46 H84 Cl Li N4 O3 Si Zr, 0.5(C4 H8 O)'
_chemical_formula_sum            'C48 H88 Cl Li N4 O3.5 Si Zr'
_chemical_formula_weight         938.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-01-12 deposited with the CCDC.
2015-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.0434(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.9179(11)
_cell_length_b                   10.9638(5)
_cell_length_c                   36.5714(15)
_cell_measurement_reflns_used    9253
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      21.90
_cell_measurement_theta_min      2.23
_cell_volume                     10392.1(8)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            41191
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.459
_diffrn_reflns_theta_min         1.114
_exptl_absorpt_coefficient_mu    0.328
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_correction_T_min  0.9045
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.364
_exptl_crystal_size_mid          0.318
_exptl_crystal_size_min          0.175
_refine_diff_density_max         0.773
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         10729
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0461
_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^)+(0.0598P)^2^+13.9890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1288
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7893
_reflns_number_total             10729
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00306g2.cif
_cod_data_source_block           riv1301
_cod_depositor_comments
'Adding full bibliography for 7034303--7034308.cif.'
_cod_original_formula_sum        'C48 H88 Cl Li N4 O3.50 Si Zr'
_cod_database_code               7034308
_shelx_estimated_absorpt_t_min   0.890
_shelx_estimated_absorpt_t_max   0.945
_shelxl_version_number           2013-4
_shelx_res_checksum              82612