Pyridazine-bridged expanded rosarin and semi-rosarinogen.
Xu, Kui; Zhang, Xiaoshuai; Liu, Guopeng; Ma, Wanzun; Yin, Yu; Yin, Ying; Chen, Xi; Zhao, Xinyun; Sessler, Jonathan L.; Zhang, Zhan; Chemical communications (Cambridge, England) 57 (2021) 1486–1489; doi:10.1039/d0cc07433k

data_7127783
_publ_section_title
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 Pyridazine-bridged expanded rosarin and semi-rosarinogen.
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_journal_issue                   12
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1486
_journal_page_last               1489
_journal_paper_doi               10.1039/d0cc07433k
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         '3(C H Cl3), C81 H84 N12'
_chemical_formula_sum            'C84 H87 Cl9 N12'
_chemical_formula_weight         1583.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_block_doi                 10.5517/ccdc.csd.cc265fys
_audit_creation_date             2020-08-20
_audit_creation_method
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_audit_update_record
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2020-12-01 deposited with the CCDC.	2021-01-08 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 94.8920(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.8725(2)
_cell_length_b                   16.7463(3)
_cell_length_c                   42.5496(8)
_cell_measurement_reflns_used    9286
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      54.93
_cell_measurement_theta_min      3.630
_cell_volume                     8428.9(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      170.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            89206
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.949
_diffrn_reflns_theta_min         3.299
_exptl_absorpt_coefficient_mu    2.041
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.5046
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 (Bruker,2016/2) '
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       prism
_exptl_crystal_F_000             3312
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.108
_refine_diff_density_min         -1.211
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     970
_refine_ls_number_reflns         15960
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0768
_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^)+(0.1171P)^2^+13.8389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2152
_refine_ls_wR_factor_ref         0.2260
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12997
_reflns_number_total             15960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc07433k2.cif
_cod_data_source_block           mjl18339_0m_pl
_cod_depositor_comments          'Adding full bibliography for 7127783.cif.'
_cod_database_code               7127783
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.792
_olex2_refinement_description
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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
2. Restrained distances
 N3-H3 = N12-H12 = N7-H7
 0.86 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(Cl3) \\sim Ueq, Uanis(Cl12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C4(H4)
4.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C32(H32A,H32B), C42(H42A,H42B), C44(H44A,H44B), C50(H50A,
 H50B), C52(H52A,H52B), C62(H62A,H62B), C64(H64A,H64B), C70(H70A,H70B),
 C72(H72A,H72B), C82(H82A,H82B), C84(H84A,H84B)
4.c Aromatic/amide H refined with riding coordinates:
 C26(H26), C27(H27), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39),
 C46(H46), C47(H47), C55(H55), C56(H56), C57(H57), C58(H58), C59(H59), C66(H66),
  C67(H67), C75(H75), C76(H76), C77(H77), C78(H78), C79(H79)
4.d Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C43(H43A,H43B,H43C), C45(H45A,H45B,
 H45C), C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C63(H63A,H63B,H63C), C65(H65A,
 H65B,H65C), C71(H71A,H71B,H71C), C73(H73A,H73B,H73C), C83(H83A,H83B,H83C),
 C85(H85A,H85B,H85C)
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_smtbx_masks_special_details
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Every molecule of compound (I) was distributed with 
another 0.6 chloroform molecule according to the 
residual electron density of ~148 e per unit 
cell and our crystallization condition. Then, 
the pratical formula should 
be (C~81~H~84~N~12~).3.6(C H Cl~3~).
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_olex2_submission_special_instructions 'No special instructions were received'