Dinuclear Cationic Zirconium Hydrides Stabilized by theN,N-Dibenzylcyclam Ancillary Ligand
Munhá, Rui F.; Ballmann, Joachim; Veiros, Luis F.; Patrick, Brian O.; Fryzuk, Michael D.; Martins, Ana M.; Organometallics 31 (2012) 4937–; doi:10.1021/om300504q

data_4078895
_publ_section_title
;
 Dinuclear Cationic Zirconium Hydrides Stabilized by theN,N-Dibenzylcyclam
 Ancillary Ligand
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              4937
_journal_paper_doi               10.1021/om300504q
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C62 H102 B N8 O2 Zr2'
_chemical_formula_weight         1184.77
_chemical_name_systematic
; 
 ? 
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.0336(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.7463(4)
_cell_length_b                   16.0456(4)
_cell_length_c                   25.7734(7)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.05
_cell_measurement_theta_min      2.30
_cell_volume                     6898.7(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'area detector'
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            32386
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         28.15
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.345
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.838
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS,Sheldrick(2008)
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2524
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.435
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         8396
_refine_ls_number_restraints     690
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0985P)^2^+10.1732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1645
_refine_ls_wR_factor_ref         0.1793
_reflns_number_gt                6254
_reflns_number_total             8396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300504q_si_002.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_atom_sites_solution_hydrogens' value 'diff&geom' was changed to
'mixed'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4078895