Facile synthesis of a B,D-tetradehydrocorrin and rearrangement to bacteriochlorins
Aravindu, Kunche; Krayer, Michael; Kim, Han-Je; Lindsey, Jonathan S.; New Journal of Chemistry 35 (2011) 1376–; doi:10.1039/c1nj20027e

data_7052661
_publ_section_title
;
 Facile synthesis of a B,D-tetradehydrocorrin and rearrangement to
 bacteriochlorins
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1376
_journal_paper_doi               10.1039/c1nj20027e
_journal_volume                  35
_journal_year                    2011
_chemical_formula_sum            'C49 H62 N4 O2'
_chemical_formula_weight         739.03
_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                 102.583(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0127(9)
_cell_length_b                   9.5391(5)
_cell_length_c                   26.1916(13)
_cell_measurement_reflns_used    9976
_cell_measurement_temperature    110
_cell_measurement_theta_max      24.52
_cell_measurement_theta_min      2.28
_cell_volume                     4148.4(4)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex2
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  XL
_computing_structure_solution    XS
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius Kappa Axis X8 Apex2'
_diffrn_measurement_method       'omega and phi 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  0.0641
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            58925
_diffrn_reflns_theta_full        25.74
_diffrn_reflns_theta_max         25.74
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.9986
_exptl_absorpt_correction_T_min  0.9732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.597
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         7899
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1499
_refine_ls_R_factor_gt           0.0939
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1458P)^2^+6.5854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2490
_refine_ls_wR_factor_ref         0.2866
_reflns_number_gt                4805
_reflns_number_total             7899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1nj20027e.txt
_cod_data_source_block           x05058
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7052661