Hybrid Macrocycles of Subporphyrins and Triphyrins.
Kumar, Ankit; Rajeswara Rao, M.; Lee, Way-Zen; Ravikanth, Mangalampalli; Organic letters 19 (2017) 5924–5927; doi:10.1021/acs.orglett.7b02919

data_1547763
_publ_section_title
;
 Hybrid Macrocycles of Subporphyrins and Triphyrins.
;
_journal_issue                   21
_journal_name_full               'Organic letters'
_journal_page_first              5924
_journal_page_last               5927
_journal_paper_doi               10.1021/acs.orglett.7b02919
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C43 H25 F5 N2 S'
_chemical_formula_sum            'C43 H25 F5 N2 S'
_chemical_formula_weight         696.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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     dual
_audit_creation_date             2017-10-09
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.749(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.947(2)
_cell_length_b                   10.5971(10)
_cell_length_c                   22.6459(17)
_cell_measurement_reflns_used    1715
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.5650
_cell_measurement_theta_min      2.9770
_cell_volume                     7073.2(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w   -135.00 -11.00   1.00    8.00    -- -101.00  72.00-108.00  124
  2  \w   -122.00  39.00   1.00    8.00    --  -32.00   0.00 -36.00  161
  3  \w   -191.00 -76.00   1.00    8.00    -- -101.00   0.00  36.00  115
  4  \w    -91.00 -24.00   1.00    8.00    -- -101.00  72.00 108.00   67
  5  \w   -189.00-121.00   1.00    8.00    -- -101.00 -72.00  36.00   68
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0041378000
_diffrn_orient_matrix_UB_12      0.0078897000
_diffrn_orient_matrix_UB_13      0.0659935000
_diffrn_orient_matrix_UB_21      -0.0401097000
_diffrn_orient_matrix_UB_22      0.0921050000
_diffrn_orient_matrix_UB_23      -0.0232849000
_diffrn_orient_matrix_UB_31      -0.0332338000
_diffrn_orient_matrix_UB_32      -0.1122271000
_diffrn_orient_matrix_UB_33      -0.0143667000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1545
_diffrn_reflns_av_unetI/netI     0.2182
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            11459
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        64.978
_diffrn_reflns_theta_max         64.978
_diffrn_reflns_theta_min         2.999
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       plate
_exptl_crystal_F_000             2864
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.044
_refine_diff_density_max         0.610
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         5944
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.2514
_refine_ls_R_factor_gt           0.1596
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3817
_refine_ls_wR_factor_ref         0.4582
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2057
_reflns_number_total             5944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b02919_si_005.cif
_cod_data_source_block           mr-ak-dbtm_cu
_cod_depositor_comments
'Adding full bibliography for 1547760--1547763.cif.'
_cod_original_cell_volume        7073.2(11)
_cod_database_code               1547763
_reflns_odcompleteness_completeness 93.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.18
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C8(H8), C19(H19), C42(H42), C38(H38), C41(H41), C13(H13), C31(H31),
 C20(H20), C14(H14), C2(H2), C12(H12), C3(H3), C39(H39), C7(H7), C32(H32),
 C35(H35), C34(H34), C18(H18)
2.b Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C), C36(H36A,H36B,H36C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.783
_oxdiff_exptl_absorpt_empirical_full_min 0.531