Spacially Confined M2Centers (M = Fe, Co, Ni, Zn) on a Sterically Bulky Binucleating Support: Synthesis, Structures and Ethylene Oligomerization Studies
Champouret, Yohan D. M.; Fawcett, John; Nodes, William J.; Singh, Kuldip; Solan, Gregory A.; Inorganic Chemistry 45 (2006) 9890–9900; doi:10.1021/ic061286x

data_4333032
_publ_section_title
;
 Spacially Confined M2Centers (M = Fe, Co, Ni, Zn) on a Sterically Bulky
 Binucleating Support:&#x00A0; Synthesis, Structures and Ethylene
 Oligomerization Studies
;
_journal_issue                   24
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9890
_journal_page_last               9900
_journal_paper_doi               10.1021/ic061286x
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         '(C46 H52 Br3 N5 Ni2 O) 3(C2 H3 N) 0.5(H2 O)'
_chemical_formula_sum            'C52 H62 Br3 N8 Ni2 O1.5'
_chemical_formula_weight         1180.25
_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                65.587(4)
_cell_angle_beta                 78.435(4)
_cell_angle_gamma                66.968(4)
_cell_formula_units_Z            2
_cell_length_a                   13.267(3)
_cell_length_b                   14.100(3)
_cell_length_c                   16.802(4)
_cell_measurement_reflns_used    849
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.98
_cell_measurement_theta_min      3.08
_cell_volume                     2631.1(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.1077
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20612
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    3.039
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
absorption correction based on 7603 reflections(SADABS); Rint 0.1027 before 
cOrrection and 0.0370 after. 

;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1206
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.144
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.890
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         10213
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.890
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0378P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0916
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                6369
_reflns_number_total             10213
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061286xsup5.cif
_cod_data_source_block           05060
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 
;
_cod_original_cell_volume        2631.1(11)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C52 H62 Br3 N8 Ni2 O1.50'
_cod_database_code               4333032