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_7713954
_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         'C32 H25 N7 O2'
_chemical_formula_sum            'C32 H25 N7 O2'
_chemical_formula_weight         539.59
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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             2023-09-07
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-09-07 deposited with the CCDC.	2023-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                64.991(2)
_cell_angle_beta                 86.277(2)
_cell_angle_gamma                73.1680(10)
_cell_formula_units_Z            2
_cell_length_a                   8.32580(10)
_cell_length_b                   13.2735(2)
_cell_length_c                   13.4369(2)
_cell_measurement_reflns_used    22718
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.1200
_cell_measurement_theta_min      2.5300
_cell_volume                     1285.23(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.15 (Rigaku OD, 2018)'
_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_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -11.00  83.00   0.50   20.08    --    9.19  57.00 -60.00  188
  2  \w    -10.00  89.00   0.50   20.08    --    9.19  37.00-150.00  198
  3  \w    -19.00  77.00   0.50   20.08    --    9.19  77.00-180.00  192
  4  \w     -2.00  48.00   0.50   20.08    --    9.19 -99.00-150.00  100
  5  \w     -2.00  48.00   0.50   20.08    --    9.19 -99.00  90.00  100
  6  \w    -14.00  86.00   0.50   20.08    --    9.19  19.00 120.00  200
  7  \w    -72.00 -20.00   0.50   20.08    --  -10.75 140.00 -34.00  104
  8  \w    -66.00 -15.00   0.50   20.08    --  -10.75 130.00 152.00  102
  9  \w    -71.00  27.00   0.50   20.08    --    9.19 -19.00 150.00  196
 10  \w    -65.00  29.00   0.50   20.08    --    9.19 -57.00  30.00  188
 11  \w    -65.00  29.00   0.50   20.08    --    9.19 -57.00 -90.00  188
 12  \w    -65.00  29.00   0.50   20.08    --    9.19 -57.00   0.00  188
 13  \w    -85.00  10.00   0.50   20.08    --  -10.75 -57.00 -30.00  190
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0701301000
_diffrn_orient_matrix_UB_12      -0.0025615000
_diffrn_orient_matrix_UB_13      -0.0251485000
_diffrn_orient_matrix_UB_21      -0.0291936000
_diffrn_orient_matrix_UB_22      -0.0274971000
_diffrn_orient_matrix_UB_23      0.0526223000
_diffrn_orient_matrix_UB_31      -0.0467609000
_diffrn_orient_matrix_UB_32      0.0550742000
_diffrn_orient_matrix_UB_33      -0.0025159000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_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            45707
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.282
_diffrn_reflns_theta_min         2.561
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.15 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_description       needle
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details
;
 Flack x determined using 4596 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.7(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         12387
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0637P)^2^+0.2992P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.949
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.948
_reflns_number_gt                10739
_reflns_number_total             12387
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02486e2.cif
_cod_data_source_block           sjkc19rr11
_cod_database_code               7713954
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C32 N7 O2 H20'
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.973
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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. Shared sites
{N55, C55A}
{N11, C11A}
{N51A, C51}
{C10A, N10}
3. Uiso/Uaniso restraints and constraints
Uanis(C29A) = Uanis(C29B)
Uanis(C30B) = Uanis(C30A)
Uanis(N7A) = Uanis(N7B) = Uanis(N6A) = Uanis(N6B) = Uanis(N5A) = Uanis(N5B)
Uanis(N55) = Uanis(C55A)
Uanis(N11) = Uanis(C11A)
Uanis(N51A) = Uanis(C51)
Uanis(C10A) = Uanis(N10)
4. Others
 Fixed Sof: N11(0.5) N55(0.5) H50A(0.5) H50(0.5) C51(0.5) H51(0.5) N10(0.5)
 H53A(0.5) H53(0.5) H58(0.5) H58A(0.5) H28(0.6) H28A(0.4) N6A(0.6) H56A(0.5)
 H56(0.5) N7A(0.6) C29A(0.6) H29A(0.6) N5A(0.6) C30A(0.6) H30A(0.6) H30B(0.6)
 H30C(0.6) C29B(0.4) H29B(0.4) C30B(0.4) H30D(0.4) H30E(0.4) H30F(0.4) N7B(0.4)
 N6B(0.4) N5B(0.4) C55A(0.5) H55A(0.5) C11A(0.5) H11A(0.5) N51A(0.5) C10A(0.5)
 H10A(0.5)
5.a Ternary CH refined with riding coordinates:
 C61(H61), C29A(H29A), C29B(H29B)
5.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C7(H7), C39(H39), C20(H20), C50(H50A), C50(H50), C57(H57),
 C0AA(H0AA), C8(H8), C16(H16), C19(H19), C40(H40), C51(H51), C3(H3), C15(H15),
 C60(H60), C26(H26), C18(H18), C33(H33), C25(H25), C45(H45), C36(H36),
 C53(H53A), C53(H53), C44(H44), C58(H58), C58(H58A), C28(H28), C28(H28A),
 C34(H34), C23(H23), C24(H24), C4(H4), C42(H42), C1AA(H1AA), C56(H56A),
 C56(H56), C10(H10), C35(H35), C48(H48), C55A(H55A), C11A(H11A), C10A(H10A)
5.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C64(H64A,H64B,H64C), C62(H62A,H62B,H62C), C30A(H30A,H30B,
 H30C), C30B(H30D,H30E,H30F)
;
_shelx_res_checksum              1856
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.147
_oxdiff_exptl_absorpt_empirical_full_min 0.827