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_4134343
_publ_section_title
;
 TetrazineBox: A Structurally Transformative ToolBox.
;
_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), 2(C22 H18 N4), 2(C H1.5 N0.5)'
_chemical_formula_sum            'C46 H39 F24 N9 P4'
_chemical_formula_weight         1297.74
_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             2017-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                106.7410(10)
_cell_angle_beta                 99.5330(10)
_cell_angle_gamma                110.0920(10)
_cell_formula_units_Z            2
_cell_length_a                   13.3898(4)
_cell_length_b                   14.5809(4)
_cell_length_c                   15.0625(4)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.56
_cell_measurement_theta_min      3.21
_cell_volume                     2527.68(13)
_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      99.97
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0676
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            58261
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        66.976
_diffrn_reflns_theta_max         66.98
_diffrn_reflns_theta_min         3.21
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.626
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0739 before and 0.0523 after correction.
The Ratio of minimum to maximum transmission is 0.7763.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       plate
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     795
_refine_ls_number_reflns         8893
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0607
_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^)+(0.0800P)^2^+3.6463P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1629
_refine_ls_wR_factor_ref         0.1704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7821
_reflns_number_total             8893
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01114_si_006.cif
_cod_data_source_block           7PF6
_cod_original_cell_volume        2527.68(12)
_cod_database_code               4134343
_shelx_estimated_absorpt_t_max   0.750
_shelx_estimated_absorpt_t_min   0.513
_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
2. Restrained distances
 C1-N1AA = N3-C4
 1.16 with sigma of 0.02
 C1-C1_$1
 1.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Fixed Sof: F00V(0.5) F01O(0.5) F021(0.5) F023(0.5) F1(0.5) F2(0.5) F3(0.5)
 F4(0.5) H1A(0.5) H1B(0.5) H1C(0.5) N1AA(0.5) N3(0.5) H4A(0.5) H4B(0.5) H4C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C01L(H01A,H01B), C01S(H01C,H01F), C026(H02A,H02B), C028(H02C,H02D)
5.b Aromatic/amide H refined with riding coordinates:
 C018(H018), C019(H019), C01A(H01G), C01C(H01I), C01D(H01D), C01E(H01E),
 C01G(H01J), C01H(H01H), C01I(H01L), C01J(H01M), C01K(H01K), C01M(H01O),
 C01N(H01N), C01P(H01P), C01Q(H01Q), C01R(H01R), C01T(H01T), C01U(H01U),
 C01V(H01V), C01W(H01W), C01X(H01X), C01Y(H01Y), C01Z(H01Z), C020(H020),
 C022(H022), C024(H024), C025(H025), C027(H027)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              15345
_shelx_hkl_checksum              66221
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'