Geometric deconstruction of core and electron activation of a π-system in a series of deformed porphyrins: mimics of heme.
Liu, Qiuhua; Zhang, Jinjin; Tang, Min; Yang, Yan; Zhang, Jian; Zhou, Zaichun; Organic & biomolecular chemistry 16 (2018) 7725–7736; doi:10.1039/c8ob01959b

data_7156462
_publ_section_title
;
 Geometric deconstruction of core and electron activation of a \p-system
 in a series of deformed porphyrins: mimics of heme.
;
_journal_issue                   41
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              7725
_journal_page_last               7736
_journal_paper_doi               10.1039/c8ob01959b
_journal_volume                  16
_journal_year                    2018
_chemical_formula_moiety         'C68 H74 N4 O4, C6 H5 N O2'
_chemical_formula_sum            'C74 H79 N5 O6'
_chemical_formula_weight         1134.42
_chemical_name_systematic        DL4TtPP
_chemical_properties_physical    Photo-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-09-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-20 deposited with the CCDC.
2018-09-27 downloaded from the CCDC.
;
_cell_angle_alpha                114.288(13)
_cell_angle_beta                 91.261(2)
_cell_angle_gamma                94.928(15)
_cell_formula_units_Z            2
_cell_length_a                   14.0320(14)
_cell_length_b                   16.4690(18)
_cell_length_c                   16.5250(18)
_cell_measurement_reflns_used    4282
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      72.30
_cell_measurement_theta_min      27.60
_cell_volume                     3461.0(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'Rigaku Saturn944 CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0742
_diffrn_reflns_av_unetI/netI     0.0649
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38669
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        67.750
_diffrn_reflns_theta_max         72.959
_diffrn_reflns_theta_min         2.940
_exptl_absorpt_coefficient_mu    0.543
_exptl_absorpt_correction_T_max  0.9086
_exptl_absorpt_correction_T_min  0.8899
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.089
_exptl_crystal_description       prism
_exptl_crystal_F_000             1212
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform, methanol'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_platon_squeeze_details
;
;
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.0118(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         12857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1401P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10289
_reflns_number_total             12857
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ob01959b2.cif
_cod_data_source_block           DL4TtPP
_cod_depositor_comments
'Adding full bibliography for 7156452--7156463.cif.'
_cod_database_code               7156462
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.909
_shelx_estimated_absorpt_t_min   0.890
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H) groups
2. Others
 Fixed Sof: H1(0.5) H2(0.5) H3(0.5) H4(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C55(H55A,
 H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,H58B)
3.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N3(H3), N4(H4), C2(H2A), C3(H3A), C7(H7), C8(H8), C12(H12), C13(H13),
 C17(H17), C18(H18), C23(H23), C25(H25), C26(H26), C37(H37), C39(H39), C40(H40),
  C47(H47), C49(H49), C50(H50), C61(H61), C63(H63), C64(H64), C70(H70),
 C71(H71), C72(H72), C73(H73), C74(H74)
3.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C42(H42A,H42B,
 H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C52(H52A,H52B,H52C), C53(H53A,
 H53B,H53C), C54(H54A,H54B,H54C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C),
 C68(H68A,H68B,H68C)
;
_shelx_res_checksum              57650
_olex2_submission_special_instructions 'No special instructions were received'