Synthesis, mechanism and ethylene polymerization catalysis of Ge(IV), Sn(II) and Zr(IV) complexes derived from substituted β-diketiminates
Xiao, Xia; Hao, Xiaomin; Bai, Jianliang; Chao, Jianbin; Cao, Wei; Chen, Xia; RSC Adv.  (2016) –; doi:10.1039/C6RA11097E

data_7225507
_publ_section_title
;
 Synthesis, mechanism and ethylene polymerization catalysis of Ge(IV),
 Sn(II) and Zr(IV) complexes derived from substituted \b-diketiminates
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C6RA11097E
_journal_year                    2016
_chemical_formula_sum            'C13 H33 Cl N4 Si2 Sn'
_chemical_formula_weight         455.75
_chemical_name_systematic
; 
 ? 
;
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-05-31 deposited with the CCDC.
2016-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.121(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.7137(17)
_cell_length_b                   15.426(2)
_cell_length_c                   11.7657(17)
_cell_measurement_reflns_used    4254
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      16.470
_cell_measurement_theta_min      2.183
_cell_volume                     2125.6(5)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'oil sealed '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0427
_diffrn_reflns_av_sigmaI/netI    0.0450
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8605
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.18
_diffrn_standards_decay_%        4.41
_exptl_absorpt_coefficient_mu    1.441
_exptl_absorpt_correction_T_max  0.7615
_exptl_absorpt_correction_T_min  0.7615
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.580
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3697
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0517
_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^)+(0.1000P)^2^+9.7463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1577
_refine_ls_wR_factor_ref         0.1745
_reflns_number_gt                3209
_reflns_number_total             3697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6ra11097e1.cif
_cod_data_source_block           hs0350p
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7225507