Stepwise deprotonation of truxene: structures, metal complexation, and charge-dependent optical properties.
Guo, Yumeng; Torchon, Herdya S.; Zhu, Yikun; Wei, Zheng; Zhang, Zhenyi; Han, Haixiang; Petrukhina, Marina A.; Zhou, Zheng; Chemical science 14 (2023) 13219–13227; doi:10.1039/d3sc04885c

data_1570222
_publ_section_title
;
 Stepwise deprotonation of truxene: structures, metal complexation, and
 charge-dependent optical properties.
;
_journal_issue                   45
_journal_name_full               'Chemical science'
_journal_page_first              13219
_journal_page_last               13227
_journal_paper_doi               10.1039/d3sc04885c
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         '2(C20 H40 Na O8), C27 H16'
_chemical_formula_sum            'C67 H96 Na2 O16'
_chemical_formula_weight         1203.41
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-11-18
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2022.11.02 svn.ra8b101fa for OlexSys, GUI svn.r6635)
;
_audit_update_record
;
2023-08-18 deposited with the CCDC.	2023-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6941(2)
_cell_length_b                   21.0294(3)
_cell_length_c                   22.7326(2)
_cell_measurement_reflns_used    3116
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      50.29
_cell_measurement_theta_min      3.85
_cell_volume                     6546.50(15)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100 CMOS'
_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  0.0904
_diffrn_reflns_av_unetI/netI     0.1277
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27814
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        63.802
_diffrn_reflns_theta_max         63.802
_diffrn_reflns_theta_min         2.862
_diffrn_source_current           1.1
_diffrn_source_power             0.05500000000000001
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.9635
_exptl_absorpt_correction_T_min  0.8524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1503 before and 0.0862 after correction.
 
For component 2:
 wR2(int) was 0.1577 before and 0.1017 after correction.
 The Ratio of minimum to maximum transmission is 0.61.

Final HKLF 4 output contains 65738 reflections, Rint = 0.0949
 (27818 with I > 3sig(I), Rint = 0.0701)
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_description       block
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.143
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.2(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.278
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     743
_refine_ls_number_reflns         10347
_refine_ls_number_restraints     812
_refine_ls_restrained_S_all      1.302
_refine_ls_R_factor_all          0.2595
_refine_ls_R_factor_gt           0.1750
_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          0.3973
_refine_ls_wR_factor_ref         0.4689
_reflns_Friedel_coverage         0.763
_reflns_Friedel_fraction_full    0.923
_reflns_Friedel_fraction_max     0.923
_reflns_number_gt                4174
_reflns_number_total             10347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc04885c2.cif
_cod_data_source_block           cu_20221116_gym_5_0m_a
_cod_depositor_comments
'Adding full bibliography for 1570220--1570225.cif.'
_cod_original_cell_volume        6546.51(15)
_cod_database_code               1570222
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.924
_shelx_estimated_absorpt_t_min   0.794
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.8(5)
 0.2(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Restrained distances
 C45-C3
 2.4 with sigma of 0.02
 C3-C01I = C45-C4 = C4-C01I
 1.54 with sigma of 0.02
 C1-C00Y = C2-C1 = C011-C00Y
 1.54 with sigma of 0.02
 C01Y-C01S = C00S-C00J = C014-C013 = C00W-C00P = C00V-C00T = C024-C01F
 1.54 with sigma of 0.02
 O0C-C014 = O0C-C00P = O08-C00W = O08-C00V = O0G-C00T = O0G-C024 = O00I-C01F =
 O00I-C01Y = O0E-C01S = O0E-C00S = O05-C00J = O05-C013
 1.43 with sigma of 0.02
 C01Y-C01F
 2.4 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 2A
O03 \\sim C01I \\sim C3 \\sim C4 \\sim C45: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 C63, C00Q, C010, C01L, C019, C025, C012, C020, C01Q, C58, C01K, C02B, C72,
 C01M, C023, C01V, C028, C01R, C01D, C027, C01B, C02A, C01A, C01O, C34, C10, C76
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C00J(H00A,H00B), C00K(H00Q,H00R), C00L(H00S,H00T), C1(H1A,H1B), C00N(H00U,
 H00V), C00O(H00W,H00X), C00P(H00C,H00D), C2(H2A,H2B), C00S(H00E,H00F),
 C00T(H00G,H00H), C00U(H00I,H00J), C00V(H00K,H00L), C00W(H00M,H00N), C00X(H00Y,
 H), C00Y(H00O,H00P), C00Z(H00Z,HA), C011(H01A,H01B), C013(H01C,H01D),
 C014(H01E,H01F), C015(H01Q,H01R), C016(H01G,H01H), C017(H01S,H01T), C01C(H01U,
 H01V), C01F(H01I,H01J), C01G(H01W,H01X), C01H(H01Y,HB), C01I(H01Z,HC),
 C01J(H01,HD), C01P(H1,HE), C01S(H01K,H01L), C01T(H2,HF), C01W(H3,HG),
 C01X(H01M,H01N), C01Y(H01O,H01P), C01Z(H4,HH), C020(H02E,H02F), C024(H02A,
 H02B), C026(H02C,H02D), C3(H3A,H3B), C4(H4A,H4B), C45(H45A,H45B)
6.b Aromatic/amide H refined with riding coordinates:
 C00Q(H00), C010(H010), C019(H019), C01O(H5), C10(H10), C76(H76), C63(H63),
 C01Q(H6), C027(H027), C34(H34), C01B(H7), C028(H028), C02A(H02G), C58(H58)
6.c Fitted hexagon refined as free rotating group:
 C01A(C01D,C01O,C10,C76,C63), C01V(C027,C34,C01B,C028,C72)
;
_shelx_res_checksum              15046
_shelx_hkl_checksum              71560
_olex2_submission_special_instructions 'No special instructions were received'