Northern-Southern Route to Synthetic Bacteriochlorins.
Liu, Yizhou; Lindsey, Jonathan S.; The Journal of organic chemistry 81 (2016) 11882–11897; doi:10.1021/acs.joc.6b02334

data_4037440
_publ_section_title
;
 Northern-Southern Route to Synthetic Bacteriochlorins.
;
_journal_issue                   23
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11882
_journal_page_last               11897
_journal_paper_doi               10.1021/acs.joc.6b02334
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C44 H46 N4 O4'
_chemical_formula_sum            'C44 H46 N4 O4'
_chemical_formula_weight         694.85
_chemical_name_systematic
;
'2,12-Diethoxycarbonyl-8,8,18,18-tetramethyl-5,15-di-p-tolylbacteriochlorin'
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                77.68(3)
_cell_angle_beta                 83.36(5)
_cell_angle_gamma                75.72(3)
_cell_formula_units_Z            1
_cell_length_a                   7.934(10)
_cell_length_b                   8.377(10)
_cell_length_c                   14.692(17)
_cell_measurement_reflns_used    8532
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      28.4719
_cell_measurement_theta_min      2.5802
_cell_volume                     922.5(19)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius X8 Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24610
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.56
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.95
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS Inc.)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             370
_exptl_crystal_size_max          0.512
_exptl_crystal_size_mid          0.304
_exptl_crystal_size_min          0.114
_refine_diff_density_max         1.501
_refine_diff_density_min         -0.437
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         4575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.1125P)^2^+1.9751P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2129
_refine_ls_wR_factor_ref         0.2320
_reflns_number_gt                3519
_reflns_number_total             4575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b02334_si_005.cif
_cod_data_source_block           global
_cod_database_code               4037440
_shelx_res_checksum              33070
_shelx_hkl_checksum              90816