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_4134346
_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), C40 H32 N12, 7(C2 H3 N)'
_chemical_formula_sum            'C54 H53 F24 N19 P4'
_chemical_formula_weight         1548.03
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-16
_audit_creation_method
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Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
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_cell_angle_alpha                90
_cell_angle_beta                 90.954(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4620(7)
_cell_length_b                   20.4049(7)
_cell_length_c                   19.1126(7)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.99
_cell_measurement_theta_min      3.17
_cell_volume                     6809.1(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      100.05
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0476
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            42608
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        65.085
_diffrn_reflns_theta_max         65.085
_diffrn_reflns_theta_min         3.168
_exptl_absorpt_coefficient_mu    2.094
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6142
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0822 before and 0.0555 after correction.
The Ratio of minimum to maximum transmission is 0.8161.
The \l/2 correction factor is Not present.
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_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_description       block
_exptl_crystal_F_000             3144
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.089
_refine_diff_density_max         1.199
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     917
_refine_ls_number_reflns         11524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0628
_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^)+(0.0910P)^2^+9.9100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1657
_refine_ls_wR_factor_ref         0.1770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9251
_reflns_number_total             11524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01114_si_002.cif
_cod_data_source_block           4PF6
_cod_original_cell_volume        6809.1(5)
_cod_database_code               4134346
_shelx_shelxl_version_number     2014/7
_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:
 C01S(H01A,H01B), C01X(H01G,H01I), C026(H02A,H02B), C02A(H02C,H02D)
2.b Aromatic/amide H refined with riding coordinates:
 C01C(H01C), C01D(H01D), C01E(H01E), C01F(H01F), C01H(H01H), C01J(H01J),
 C01K(H01K), C01L(H01L), C01M(H01M), C01O(H01O), C01P(H01P), C01R(H01R),
 C01T(H01T), C01U(H01U), C01V(H01V), C01Y(H01Y), C020(H020), C021(H021),
 C022(H022), C023(H023), C025(H025), C027(H027), C028(H028), C029(H029)
2.c Idealised Me refined as rotating group:
 C02H(H02E,H02F,H02G), C02N(H02N,H02O,H02P), C02P(H02H,H02I,H02J), C02Q(H02Q,
 H02R,H02S), C02R(H02T,H02U,H02V), C02S(H02W,H02X,H02Y), C02T(H02K,H02L,H02M)
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_olex2_submission_special_instructions 'No special instructions were received'