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_4084447
_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
'C24 H57 N8 Si Zr2, C24 H12 B Cl8, 0.5(C6 H12),C4 H8 O'
_chemical_formula_sum            'C55 H83 B Cl8 N8 O Si Zr2'
_chemical_formula_weight         1377.23
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 100.3265(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4460(7)
_cell_length_b                   18.0452(10)
_cell_length_c                   28.4705(16)
_cell_measurement_reflns_used    6381
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.36
_cell_measurement_theta_min      2.24
_cell_volume                     6290.6(6)
_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 0.999
_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  0.0759
_diffrn_reflns_av_sigmaI/netI    0.0625
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            68037
_diffrn_reflns_theta_full        25.08
_diffrn_reflns_theta_max         25.08
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.735
_exptl_absorpt_correction_T_max  0.8097
_exptl_absorpt_correction_T_min  0.7429
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Bruker'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.503
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         11169
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0799
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0845P)^2^+3.7137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1454
_refine_ls_wR_factor_ref         0.1641
_reflns_number_gt                8054
_reflns_number_total             11169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500820k_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4084445--4084448.cif.'
_cod_original_sg_symbol_Hall     '-P 2YN'
_cod_original_sg_symbol_H-M      'P 1 21/N 1'
_cod_database_code               4084447