Probing the Characteristics of Mono- or Bimetallic (Iron or Cobalt) Complexes Bearing 2,4-Bis(6-iminopyridin-2-yl)-3H-benzazepines: Synthesis, Characterization, and Ethylene Reactivity
Sun, Wen-Hua; Xing, Qifeng; Yu, Jiangang; Novikova, Elena; Zhao, Weizhen; Tang, Xiubo; Liang, Tongling; Redshaw, Carl; Organometallics 32 (2013) 2309–; doi:10.1021/om301086p

data_4080327
_publ_section_title
;
 Probing the Characteristics of Mono- or Bimetallic (Iron or Cobalt)
 Complexes Bearing 2,4-Bis(6-iminopyridin-2-yl)-3H-benzazepines:
 Synthesis, Characterization, and Ethylene Reactivity
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2309
_journal_paper_doi               10.1021/om301086p
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C48 H53 N5 O0'
_chemical_formula_weight         699.95
_chemical_name_systematic
;
 ?
;
_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                 95.64(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.531(3)
_cell_length_b                   12.245(2)
_cell_length_c                   22.444(5)
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.53
_cell_volume                     4247.7(14)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material  'SHELX97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0649
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            9651
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    0.064
_exptl_absorpt_correction_T_max  0.9891
_exptl_absorpt_correction_T_min  0.9722
_exptl_absorpt_correction_type   'Multi-scan or numerical'
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         9651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_gt           0.0683
_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^)+(0.1171P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1799
_refine_ls_wR_factor_ref         0.2109
_reflns_number_gt                4717
_reflns_number_total             9651
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om301086p_si_002.cif
_cod_data_source_block           L3
_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 
;
_cod_original_cell_volume        4247.6(15)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4080327
_refine_ls_r_factor_ref          0.1357