Coordination Chemistry of N,N,N',N'-Tetrakis(3,5-substituted benzyl-2-oxide)-2,2'-(ethylenedioxy)diethanamine Modified Group 4 Metal Alkoxides
Timothy J. Boyle; Daniel T. Yonemoto; Leigh Anna Steele; Joshua Farrell; Peter Renehan; Taylor Huhta; Inorganic Chemistry 51 (2012) 12023–12031; doi:10.1021/ic3019327

data_4330973
_publ_section_title
;
 Coordination Chemistry of N,N,N',N'-Tetrakis(3,5-substituted
 benzyl-2-oxide)-2,2'-(ethylenedioxy)diethanamine Modified Group 4 Metal
 Alkoxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12023
_journal_page_last               12031
_journal_paper_doi               10.1021/ic3019327
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C96 H152 N2 O10 Zr2'
_chemical_formula_weight         1676.64
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.242(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0838(13)
_cell_length_b                   23.7108(13)
_cell_length_c                   26.2422(15)
_cell_measurement_reflns_used    9898
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.09
_cell_measurement_theta_min      2.34
_cell_volume                     9815.7(11)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            53649
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         1.55
_exptl_absorpt_coefficient_mu    0.265
_exptl_absorpt_correction_T_max  0.8923
_exptl_absorpt_correction_T_min  0.7703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.135
_exptl_crystal_description       prism
_exptl_crystal_F_000             3608
_exptl_crystal_size_max          1.04
_exptl_crystal_size_mid          0.74
_exptl_crystal_size_min          0.44
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.981
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         12518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0680
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.003
_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^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1171
_refine_ls_wR_factor_ref         0.1498
_reflns_number_gt                9212
_reflns_number_total             12518
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3019327_si_001_4.cif
_cod_data_source_block           aml11sp281tjb
_cod_database_code               4330973