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_4028089
_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            'C47 H38 N4 O5 Zn'
_chemical_formula_weight         804.18
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.9920(10)
_cell_angle_beta                 96.5610(10)
_cell_angle_gamma                97.7270(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5921(4)
_cell_length_b                   12.9701(4)
_cell_length_c                   14.8500(5)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.19
_cell_measurement_theta_min      3.26
_cell_volume                     2192.37(12)
_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 0.947
_diffrn_measured_fraction_theta_max 0.947
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0219
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23334
_diffrn_reflns_theta_full        61.00
_diffrn_reflns_theta_max         61.00
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    1.163
_exptl_absorpt_correction_T_max  0.7434
_exptl_absorpt_correction_T_min  0.5661
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS; Sheldrick, 2004 [Sheldrick, G. M. (2004)]'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.27
_platon_squeeze_details          ' '
_refine_diff_density_max         1.736
_refine_diff_density_min         -0.441
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.968
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     522
_refine_ls_number_reflns         6348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.968
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0892P)^2^+7.4737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.1748
_reflns_number_gt                6109
_reflns_number_total             6348
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo400031r_si_004.cif
_cod_data_source_block           p1
_cod_original_cell_volume        2192.36(12)
_cod_database_code               4028089