NCN Trianionic Pincer Ligand Precursors: Synthesis of Bimetallic, Chelating Diamide, and Pincer Group IV Complexes
Soumya Sarkar; Kevin P. McGowan; Jeffrey A. Culver; Adam R. Carlson; Jürgen Koller; Andrew J. Peloquin; Melanie K. Veige; Khalil A. Abboud; Adam S. Veige; Inorganic Chemistry 49 (2010) 5143–5156; doi:10.1021/ic100232s

data_4315612
_publ_section_title
;
 NCN Trianionic Pincer Ligand Precursors: Synthesis of Bimetallic,
 Chelating Diamide, and Pincer Group IV Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5143
_journal_page_last               5156
_journal_paper_doi               10.1021/ic100232s
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C36 H54 N4 Zr'
_chemical_formula_weight         634.05
_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
_audit_update_record
;
2010-01-28 # Formatted by publCIF
;
_cell_angle_alpha                107.72(2)
_cell_angle_beta                 91.20(2)
_cell_angle_gamma                108.229(19)
_cell_formula_units_Z            2
_cell_length_a                   8.2682(14)
_cell_length_b                   12.2632(16)
_cell_length_c                   18.800(4)
_cell_measurement_reflns_used    236
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      2.0
_cell_volume                     1710.4(6)
_computing_cell_refinement
'Bruker SMART v5.624 & SAINT 6.36a (Bruker 1998)'
_computing_data_collection       'Bruker SMART v5.624 (Bruker 1998)'
_computing_data_reduction        'Bruker SHELXTL v6.14 (Bruker 2000)'
_computing_molecular_graphics    'Bruker SHELXTL v6.14'
_computing_publication_material  'Bruker SHELXTL v6.14'
_computing_structure_refinement  'Bruker SHELXTL v6.14'
_computing_structure_solution    'Bruker SHELXTL v6.14'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'SMART APEX II area detector'
_diffrn_measurement_method       '\w scans'
_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  0.0148
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12504
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.350
_exptl_absorpt_correction_T_max  0.9714
_exptl_absorpt_correction_T_min  0.9281
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'based on measured indexed crystal faces, Bruker SHELXTL  v6.12 (Bruker 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needles
_exptl_crystal_F_000             676
_exptl_crystal_size_max          0.258
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.768
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         7445
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0524P)^2^+2.1716P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0966
_reflns_number_gt                7081
_reflns_number_total             7445
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic100232s_si_001_09.cif
_cod_data_source_block           ss46
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        1710.4(5)
_cod_database_code               4315612