Neutral and Cationic Zirconium Hydrides Supported by a Dianionic (NNNN)-Type Macrocycle Ligand
Kulinna, Heiko; Spaniol, Thomas P.; Okuda, Jun; Organometallics 34 (2015) 2160–; doi:10.1021/om500820k

data_4084446
_publ_section_title
;
 Neutral and Cationic Zirconium Hydrides Supported by a Dianionic
 (NNNN)-Type Macrocycle Ligand
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2160
_journal_paper_doi               10.1021/om500820k
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C28 H68 N8 Si2 Zr2, C6 H12'
_chemical_formula_sum            'C34 H80 N8 Si2 Zr2'
_chemical_formula_weight         839.68
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 107.8020(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4480(17)
_cell_length_b                   12.9787(12)
_cell_length_c                   19.4705(19)
_cell_measurement_reflns_used    9988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.35
_cell_measurement_theta_min      2.20
_cell_volume                     4198.0(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-III (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare 1992)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker APEX-I CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         microsource
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            65391
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         31.60
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  0.8818
_exptl_absorpt_correction_T_min  0.8210
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs Bruker'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         13345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+2.0105P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                11527
_reflns_number_total             13345
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500820k_si_002.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4084445--4084448.cif.'
_cod_original_sg_symbol_Hall     '-P 2YBC'
_cod_original_sg_symbol_H-M      'P 1 21/C 1'
_cod_database_code               4084446