Group 4 Bis(pyrimidinoxide) Complexes. Investigations of Electronic Effects in Catalytic Hydroamination
Lee, Alison V.; Schafer, Laurel L.; Organometallics 25 (2006) 5249–; doi:10.1021/om060587b

data_4074369
_publ_section_title
;
 Group 4 Bis(pyrimidinoxide) Complexes. Investigations of Electronic
 Effects in Catalytic Hydroamination
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5249
_journal_paper_doi               10.1021/om060587b
_journal_volume                  25
_journal_year                    2006
_chemical_formula_moiety         'C56 H96 N10 O5 Zr2'
_chemical_formula_sum            'C56 H96 N10 O5 Zr2'
_chemical_formula_weight         1171.87
_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                 90.235(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.3557(9)
_cell_length_b                   17.0718(10)
_cell_length_c                   27.0530(13)
_cell_measurement_reflns_used    34719
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.4925
_cell_measurement_theta_min      2.331
_cell_volume                     7091.9(7)
_computing_cell_refinement       APEX-2
_computing_data_collection       APEX-2
_computing_data_reduction        APEX-2
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0928
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            97415
_diffrn_reflns_theta_full        23.08
_diffrn_reflns_theta_max         23.08
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.339
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.8314
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.098
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         3.756
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         9924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0851
_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^)+(0.1451P)^2^+53.8792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2660
_refine_ls_wR_factor_ref         0.2791
_reflns_number_gt                7777
_reflns_number_total             9924
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060587bsi20060630_064613.cif
_cod_data_source_block           ls085_0m
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               4074369