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_4084445
_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         'C18 H44 N4 Si2 Zr'
_chemical_formula_sum            'C18 H44 N4 Si2 Zr'
_chemical_formula_weight         463.97
_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                 115.034(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.4537(9)
_cell_length_b                   10.8525(7)
_cell_length_c                   18.4555(10)
_cell_measurement_reflns_used    7810
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.47
_cell_measurement_theta_min      2.44
_cell_volume                     2441.5(3)
_computing_cell_refinement       'Bruker SMART (2001)'
_computing_data_collection       'Bruker SMART (2001)'
_computing_data_reduction        'Bruker SAINT+ (1999)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'APEX Area Detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'multilayer optics'
_diffrn_radiation_source         'INCOATEC microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.0327
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            36078
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.89
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.9210
_exptl_absorpt_correction_T_min  0.8374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Bruker'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     234
_refine_ls_number_reflns         7277
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0286
_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^)+(0.0286P)^2^+0.9654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0646
_refine_ls_wR_factor_ref         0.0695
_reflns_number_gt                6082
_reflns_number_total             7277
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500820k_si_002.cif
_cod_data_source_block           1
_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               4084445