Meso-to-meso 2,5-Pyrrolylene Bridged Zig-zag Porphyrin Arrays
Song, JX; zhang, senmiao; Kim, Jun Oh; Li, Yajie; Wen, Bin; Zhou, Mingbo; Liu, Shubin; Aratani, Naoki; Xu, Ling; Kim, Dongho; Chem. Commun.  (2017) –; doi:10.1039/C7CC06793C

data_7120731
_publ_section_title
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 Meso-to-meso 2,5-Pyrrolylene Bridged Zig-zag Porphyrin Arrays
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06793C
_journal_year                    2017
_chemical_formula_moiety         'C81 H84 N8 Zn1.5'
_chemical_formula_sum            'C81 H84 N8 Zn1.5'
_chemical_formula_weight         1267.61
_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   geom
_audit_creation_date             2015-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2017-07-27 deposited with the CCDC.
2017-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                95.630(3)
_cell_angle_beta                 95.061(3)
_cell_angle_gamma                104.331(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3496(4)
_cell_length_b                   15.1615(5)
_cell_length_c                   30.0085(12)
_cell_measurement_reflns_used    5444
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.7950
_cell_measurement_theta_min      4.5140
_cell_volume                     4073.6(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  supernova
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            43065
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.399
_diffrn_reflns_theta_max         67.399
_diffrn_reflns_theta_min         4.510
_exptl_absorpt_coefficient_mu    0.891
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.033
_exptl_crystal_description       block
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.298
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         14618
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.1742
_refine_ls_R_factor_gt           0.1137
_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          0.3150
_refine_ls_wR_factor_ref         0.3688
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7397
_reflns_number_total             14618
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06793c2.cif
_cod_data_source_block           exp_19_1_smart_sq
_cod_original_formula_sum        'C81 H84 N8 Zn1.50'
_cod_database_code               7120731
_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. Uiso/Uaniso restraints and constraints
Uanis(C85) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C4(H4), N0AA(H0AA), C30(H30), C36(H36), C41(H41), C46(H46), C55(H55),
 C60(H60), C63(H63), C65(H65), C71(H71), C73(H73), C1CA(H1CA), C4CA(H4CA),
 C0CA(H0CA), C2CA(H2CA), C22(H22), C29(H29), C6AA(H6AA), C33(H33), C0BA(H0BA),
 C1AA(H1AA), C52(H52), C76(H76), C90(H90), C6(H6), C8(H8), C10(H10), C11(H11),
 C13(H13)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1BA(H1BA,H1BB,H1BC), C2BA(H2BA,H2BB,H2BC), C38(H38A,H38B,
 H38C), C5AA(H5AA,H5AB,H5AC), C19(H19A,H19B,H19C), C57(H57A,H57B,H57C),
 C3AA(H3AA,H3AB,H3AC), C3BA(H3BA,H3BB,H3BC), C69(H69A,H69B,H69C), C84(H84A,H84B,
 H84C), C85(H85A,H85B,H85C), C94(H94A,H94B,H94C), C9BA(H9BA,H9BB,H9BC),
 C6BA(H6BA,H6BB,H6BC), C4BA(H4BA,H4BB,H4BC), C5CA(H5CA,H5CB,H5CC), C7BA(H7BA,
 H7BB,H7BC)
;
_shelx_res_checksum              35334
_shelx_fab_checksum              98873
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'