Picolinamide as a Directing Group on Metal Sandwich Compounds: sp2 C‒H Bond Activation and sp3 C‒H Bond Oxidation
Hazra, Susanta; Deb, Mayukh; Singh, Jatinder; Elias, Anil J.; Organometallics  (2017) –; doi:10.1021/acs.organomet.7b00143

data_4087252
_publ_section_title
;
 Picolinamide as a Directing Group on Metal Sandwich Compounds: sp2 C--H
 Bond Activation and sp3 C--H Bond Oxidation
;
_journal_name_full               Organometallics
_journal_paper_doi               10.1021/acs.organomet.7b00143
_journal_year                    2017
_chemical_formula_moiety         'C29 H22 Br2 Fe N2 O'
_chemical_formula_sum            'C29 H22 Br2 Fe N2 O'
_chemical_formula_weight         630.14
_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                 90.361(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.2890(17)
_cell_length_b                   16.8883(19)
_cell_length_c                   19.721(2)
_cell_measurement_reflns_used    2402
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      18.41
_cell_measurement_theta_min      2.39
_cell_volume                     5092.0(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0707
_diffrn_reflns_av_sigmaI/netI    0.0949
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26506
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    3.756
_exptl_absorpt_correction_T_max  0.512
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.644
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2512.0
_exptl_crystal_size_max          0.245
_exptl_crystal_size_mid          0.194
_exptl_crystal_size_min          0.178
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8927
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                4467
_reflns_number_total             8959
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om7b00143_si_002.cif
_cod_data_source_block           5e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        5091.8(10)
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4087252