Oxazolochlorins. 9.meso-Tetraphenyl-2-oxabacteriochlorins and meso-Tetraphenyl-2,12/13-dioxabacteriochlorins(1)
Junichi Ogikubo; Eileen Meehan; James T. Engle; Christopher J. Ziegler; Christian Brückner; Journal of Organic Chemistry 78 (2013) 2840–2852; doi:10.1021/jo400031r

data_4028088
_publ_section_title
;
 Oxazolochlorins. 9.meso-Tetraphenyl-2-oxabacteriochlorins and
 meso-Tetraphenyl-2,12/13-dioxabacteriochlorins(1)
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              2840
_journal_page_last               2852
_journal_paper_doi               10.1021/jo400031r
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C48.5 H38.5 N4.5 O4'
_chemical_formula_weight         748.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 117.2340(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.6921(5)
_cell_length_b                   13.7480(3)
_cell_length_c                   25.7494(8)
_cell_measurement_reflns_used    9371
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.30
_cell_measurement_theta_min      3.84
_cell_volume                     7457.3(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            21363
_diffrn_reflns_theta_full        64.61
_diffrn_reflns_theta_max         64.61
_diffrn_reflns_theta_min         3.84
_exptl_absorpt_coefficient_mu    0.684
_exptl_absorpt_correction_T_max  0.9473
_exptl_absorpt_correction_T_min  0.8320
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS; Sheldrick, 2004 [Sheldrick, G. M. (2004)]'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       plate
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         6046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0516
_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^)+(0.0946P)^2^+13.1517P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1466
_refine_ls_wR_factor_ref         0.1551
_reflns_number_gt                5127
_reflns_number_total             6046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo400031r_si_003.cif
_cod_data_source_block           c2c
_cod_depositor_comments
;

2021-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C97 H77 N9 O8'
_cod_original_formula_weight         1496.68
_cod_original_formula_units_Z            4
_cod_database_code               4028088