A Novel Bis(phosphido)pyridine [PNP]2−Pincer Ligand and Its Potassium and Bis(dimethylamido)zirconium(IV) Complexes
Winston, Matthew S.; Bercaw, John E.; Organometallics 29 (2010) 6408–; doi:10.1021/om100775g

data_4067017
_publ_section_title
;
 A Novel Bis(phosphido)pyridine [PNP]2&#x2212;Pincer Ligand and Its
 Potassium and Bis(dimethylamido)zirconium(IV) Complexes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6408
_journal_paper_doi               10.1021/om100775g
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C33 H33 N3 P2 Zr, 0.25(C6 H6)'
_chemical_formula_sum            'C34.5 H34.5 N3 P2 Zr'
_chemical_formula_weight         644.31
_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                 96.280(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.1980(9)
_cell_length_b                   33.236(4)
_cell_length_c                   23.311(2)
_cell_measurement_reflns_used    9165
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.48
_cell_measurement_theta_min      2.45
_cell_volume                     6313.4(12)
_computing_cell_refinement       'Bruker SAINT-Plus v7.66A'
_computing_data_collection       'Bruker APEX2 v2009.7-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.66A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 7 settings'
_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  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0665
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            51705
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.477
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6212
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2008/2, Bruker-AXS, Madison, WI'
_exptl_crystal_colour            Orange/red
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Blade
_exptl_crystal_F_000             2660
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.692
_refine_diff_density_min         -0.913
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.255
_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     723
_refine_ls_number_reflns         10283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.255
_refine_ls_R_factor_all          0.0852
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0734
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                7388
_reflns_number_total             10283
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100775g_si_002.cif
_cod_data_source_block           msw03
_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.

'_refine_ls_weighting_scheme' value 'Sigma' changed to
'sigma' 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:

'_atom_sites_solution_primary' value 'Direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C34.50 H34.50 N3 P2 Zr'
_cod_database_code               4067017