Pitfalls in Bromination Reactions of Zinc Porphyrins: Two-Sided Ring Opening of the Porphyrin Macrocycle.
Nandi, Goutam; Titi, Hatem M.; Goldberg, Israel; Inorganic chemistry 53 (2014) 7894–; doi:10.1021/ic500468r

data_4340470
_publ_section_title
;
 Pitfalls in Bromination Reactions of Zinc Porphyrins: Two-Sided Ring
 Opening of the Porphyrin Macrocycle.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7894
_journal_paper_doi               10.1021/ic500468r
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         '2(C48 H32 Br10 N4 O4 Zn), C H2 Cl2'
_chemical_formula_sum            'C48.5 H33 Br10 Cl N4 O4 Zn'
_chemical_formula_weight         1635.65
_chemical_name_systematic
; 
 ? 
;
_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                 90.8580(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.0103(9)
_cell_length_b                   21.6959(8)
_cell_length_c                   22.7148(8)
_cell_measurement_reflns_used    13163
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      1.30
_cell_volume                     10845.9(7)
_computing_cell_refinement       'Saint, Bruker-AXS'
_computing_data_collection       'Apex2, Bruker-AXS'
_computing_data_reduction        'Saint, Bruker-AXS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean 1.75
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'ApexDuo, Bruker-AXS'
_diffrn_measurement_method       '1 deg. \f and \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  0.0887
_diffrn_reflns_av_sigmaI/netI    0.1083
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            74009
_diffrn_reflns_theta_full        25.44
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         1.30
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.916
_exptl_absorpt_correction_T_max  0.603
_exptl_absorpt_correction_T_min  0.242
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs, Bruker-AXS'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6248
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 disordered DCM of partial occupancy
;
_refine_diff_density_max         1.787
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.226
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1242
_refine_ls_number_reflns         19888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0821
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+2.2831P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1864
_reflns_number_gt                13163
_reflns_number_total             19900
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500468r_si_001.cif
_cod_data_source_block           Compound-3
_cod_depositor_comments
'Adding full bibliography for 4340468--4340471.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4340470