TetrazineBox: A Structurally Transformative ToolBox.
Guo, Qing-Hui; Zhou, Jiawang; Mao, Haochuan; Qiu, Yunyan; Nguyen, Minh T.; Feng, Yuanning; Liang, Jiaqi; Shen, Dengke; Li, Penghao; Liu, Zhichang; Wasielewski, Michael R.; Stoddart, J. Fraser; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c01114

data_4134342
_publ_section_title
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 TetrazineBox: A Structurally Transformative ToolBox.
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_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c01114
_journal_year                    2020
_chemical_formula_moiety         '4(F6 P), C44 H36 N8, 4(C2 H3 N), C16 H10'
_chemical_formula_sum            'C68 H58 F24 N12 P4'
_chemical_formula_weight         1623.14
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
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_cell_angle_alpha                74.541(3)
_cell_angle_beta                 80.014(3)
_cell_angle_gamma                63.639(2)
_cell_formula_units_Z            1
_cell_length_a                   10.4268(5)
_cell_length_b                   11.1641(5)
_cell_length_c                   17.3653(8)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.43
_cell_volume                     1742.14(14)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      101.92
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28406
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.565
_diffrn_reflns_theta_min         2.085
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6821
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0896 before and 0.0469 after correction.
The Ratio of minimum to maximum transmission is 0.9148.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       block
_exptl_crystal_F_000             826
_exptl_crystal_size_max          0.136
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.797
_refine_diff_density_min         -0.452
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         8023
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0609
_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^)+(0.0694P)^2^+3.2369P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1598
_refine_ls_wR_factor_ref         0.1699
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6442
_reflns_number_total             8023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01114_si_009.cif
_cod_data_source_block           7_Pyrene
_cod_original_cell_volume        1742.15(15)
_cod_database_code               4134342
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.970
_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.a Secondary CH2 refined with riding coordinates:
 C00R(H00A,H00B), C015(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00L(H00L), C00P(H00P), C00S(H00S), C00V(H00V), C00W(H00W),
 C00X(H00X), C00Y(H00Y), C00Z(H00Z), C010(H010), C012(H012), C013(H013),
 C014(H014), C016(H016), C01D(H01D), C01E(H01E), C01G(H01G), C01H(H01H),
 C01I(H01I)
2.c Idealised Me refined as rotating group:
 C018(H01C,H01F,H01J), C01B(H01K,H01L,H01M)
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_shelx_res_checksum              42723
_shelx_hkl_checksum              83460
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'