Remote stereocentres do not disrupt the stereochemical coupling in homochiral [M2L3] helicates and [M4L6] tetrahedra
Siddique, Rashid G.; Whittaker, Jacob J.; AL-Fayaad, Hydar; McMurtrie, John C.; Clegg, Jack Kay; Dalton Transactions  (2023) –; doi:10.1039/D3DT02486E

data_7713953
_publ_section_title
;
 Remote stereocentres do not disrupt the stereochemical coupling in
 homochiral [M2L3] helicates and [M4L6] tetrahedra
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02486E
_journal_year                    2023
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C38 H32 N10 O4'
_chemical_formula_sum            'C38 H32 N10 O4'
_chemical_formula_weight         692.73
_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             2023-07-11
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-07-11 deposited with the CCDC.	2023-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.4710(11)
_cell_length_b                   12.167(2)
_cell_length_c                   50.751(10)
_cell_measurement_reflns_used    6042
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.124
_cell_measurement_theta_min      1.721
_cell_volume                     3378.3(11)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.1433
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            42922
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.124
_diffrn_reflns_theta_max         25.124
_diffrn_reflns_theta_min         1.721
_diffrn_source                   'MX1 Australian Synchrotron'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  'not reported by XDS'
_exptl_absorpt_correction_T_min  'not reported by XDS'
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       needle
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.138
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   2(6)
_refine_ls_extinction_coef       0.032(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     475
_refine_ls_number_reflns         6042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1487
_refine_ls_R_factor_gt           0.1236
_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^+8.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3360
_refine_ls_wR_factor_ref         0.3588
_reflns_Friedel_coverage         0.707
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4451
_reflns_number_total             6042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02486e2.cif
_cod_data_source_block           p2_a_pl
_cod_depositor_comments
;

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C76 H64 N20 O8'
_cod_original_formula_weight         1385.47
_cod_original_formula_moiety         '2(C38 H32 N10 O4)'
_cod_original_formula_units_Z            2
_cod_database_code               7713953
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: -1(6)
 2(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
 C01D(H01D), C01L(H01L)
3.b Aromatic/amide H refined with riding coordinates:
 C00G(H00G), C00I(H00I), C00K(H00K), C00N(H00N), C00T(H00T), C00U(H00U),
 C00X(H00X), C00Z(H00Z), C014(H014), C01E(H01E), C01F(H01F), C01H(H01H),
 C01K(H01K), C01Q(H01Q), C01W(H01W), C01Y(H01Y), C02L(H02L), C02V(H02V)
3.c Idealised Me refined as rotating group:
 C01B(H01A,H01B,H01C), C025(H02A,H02B,H02C), C02I(H02D,H02E,H02F), C02O(H02G,
 H02H,H02I)
;
_shelx_res_checksum              24366
_olex2_submission_special_instructions 'No special instructions were received'