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_4084448
_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 H62 N8 O2 Zr2, 2(C24 H12 B Cl8)'
_chemical_formula_sum            'C76 H86 B2 Cl16 N8 O2 Zr2'
_chemical_formula_weight         1914.79
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.5515(11)
_cell_angle_beta                 66.8464(10)
_cell_angle_gamma                85.0735(11)
_cell_formula_units_Z            2
_cell_length_a                   14.8816(10)
_cell_length_b                   16.6278(11)
_cell_length_c                   17.9682(12)
_cell_measurement_reflns_used    6839
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.99
_cell_measurement_theta_min      2.28
_cell_volume                     4072.8(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0500
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            54540
_diffrn_reflns_theta_full        27.80
_diffrn_reflns_theta_max         27.80
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.832
_exptl_absorpt_correction_T_max  0.8853
_exptl_absorpt_correction_T_min  0.6762
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs Bruker'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.712
_refine_diff_density_min         -1.408
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         19198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0999P)^2^+2.8349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.1880
_reflns_number_gt                13858
_reflns_number_total             19198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500820k_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4084445--4084448.cif.'
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4084448