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_7713955
_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 ad
_chemical_formula_moiety         'C114 H96 Fe2 N30 O12, 3(B F4)'
_chemical_formula_sum            'C116 H99 B4 F16 Fe2 N31 O12'
_chemical_formula_weight         2578.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_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                 91.093(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.3794(6)
_cell_length_b                   14.7997(2)
_cell_length_c                   30.8356(5)
_cell_measurement_reflns_used    33382
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.3890
_cell_measurement_theta_min      2.0210
_cell_volume                     12036.3(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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -24.00  76.00   2.00  400.00    --   -3.05  19.00   0.00   50
  2  \w    -24.00  76.00   2.00  400.00    --   -3.05  19.00-139.00   50
  3  \w    -52.00  -8.00   2.00  400.00    --   -3.05 119.00 -98.63   22
  4  \w    -49.00  -3.00   2.00  400.00    --   -3.05 113.00  70.08   23
  5  \w    -47.00  -3.00   2.00  400.00    --   -3.05 111.00 146.39   22
  6  \w    -82.00 -10.00   2.00  400.00    --   -3.05 -19.00  53.00   36
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_unetI/netI     0.0872
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            149906
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.067
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87767
_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            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_description       block
_exptl_crystal_F_000             5296
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.200
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
 Flack x determined using 11093 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.038(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2958
_refine_ls_number_reflns         43633
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0796
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1340P)^2^+4.4240P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2020
_refine_ls_wR_factor_ref         0.2213
_reflns_Friedel_coverage         0.904
_reflns_Friedel_fraction_full    0.982
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                31760
_reflns_number_total             43633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02486e2.cif
_cod_data_source_block           sjkc19rr32a
_cod_original_cell_volume        12036.2(4)
_cod_database_code               7713955
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Shared sites
{C186, C1A}
{N54, N54A}
{C188, C1E}
{C163, C210}
3. Restrained distances
 B3-F11
 1.35 with sigma of 0.02
 F3-B1
 1.37 with sigma of 0.02
 F1-B1
 1.37 with sigma of 0.02
 B1-F2
 1.4 with sigma of 0.02
 B1-F3
 1.4 with sigma of 0.02
 B1-F4
 1.4 with sigma of 0.02
 B1-F1
 1.4 with sigma of 0.02
 C1B-C210
 1.45 with sigma of 0.02
 O18-O17
 2.2 with sigma of 0.02
 C185-C186 \\sim C185-C1A
 with sigma of 0.02
 C186-N52 \\sim C1A-N52A
 with sigma of 0.02
 C186-C187 \\sim C1A-C32A
 with sigma of 0.02
 N52-N53 \\sim N52A-N53A
 with sigma of 0.02
 N53-N54 \\sim N53A-N54A
 with sigma of 0.02
 N54-C187 \\sim N54A-C32A
 with sigma of 0.02
 C185-N52 \\sim C185-N52A
 with sigma of 0.04
 C185-C187 \\sim C185-C32A
 with sigma of 0.04
 C186-N53 \\sim C1A-N53A
 with sigma of 0.04
 C186-N54 \\sim C1A-N54A
 with sigma of 0.04
 N52-N54 \\sim N52A-N54A
 with sigma of 0.04
 N52-C187 \\sim N52A-C32A
 with sigma of 0.04
 N53-C187 \\sim N53A-C32A
 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
N57 \\sim C174 \\sim C173 \\sim C172 \\sim C171 \\sim C170: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
C163 \\sim C210 \\sim C211 \\sim C1B \\sim C212 \\sim O16 \\sim O15 \\sim O13
\\sim O14 \\sim C1C \\sim C213: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08 within 2A
Uiso(C188) = Uiso(C1E) = Uiso(C189) = Uiso(C1D) = Uiso(O17) = Uiso(O18) =
Uiso(C191) = Uiso(C190) = Uiso(O19) = Uiso(O20) = Uiso(C0AA)
Uanis(C186) = Uanis(C1A)
Uanis(N53A) = Uanis(N53)
Uanis(C186) = Uanis(N52A) = Uanis(N53) = Uanis(N54A) = Uanis(C32A)
Uanis(C186) = Uanis(C187) = Uanis(N54) = Uanis(N53) = Uanis(N52)
Uanis(N54) = Uanis(N54A)
Uanis(C176) = Uanis(C32A) = Uanis(C186) = Uanis(N52) = Uanis(N53) = Uanis(N54)
Uanis(C4) = Uanis(C3) = Uanis(C2) = Uanis(C1) = Uanis(N1) = Uanis(C5)
Uanis(C34) = Uanis(N25) = Uanis(C38) = Uanis(C37) = Uanis(C36) = Uanis(C35)
Uanis(C69) = Uanis(C70) = Uanis(N29) = Uanis(C66) = Uanis(C67) = Uanis(C68)
Uiso(C188) = Uiso(C1E)
Uiso(C1E) = Uiso(C188)
Uanis(C81) = Uanis(N3) = Uanis(C77) = Uanis(C78) = Uanis(C79) = Uanis(C80)
Uanis(N6) = Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C48) = Uanis(C47)
Uanis(C210) = Uanis(C163)
Uanis(C163) = Uanis(C210)
Uanis(C174) = Uanis(N57) = Uanis(C170) = Uanis(C171) = Uanis(C172) = Uanis(C173)
5. Others
 Fixed Sof: C210(0.5) H210(0.5) O25(0.5) O16(0.5) C212(0.5) O15(0.5) O25A(0.5)
 C186(0.5) N52(0.5) N53(0.5) N54(0.5) C187(0.5) H187(0.5) C1A(0.5) C32A(0.5)
 H32A(0.5) N54A(0.5) N53A(0.5) N52A(0.5) F3(0.75) C213(0.5) H21G(0.5) H21H(0.5)
 H21I(0.5) C190(0.75) O20(0.75) C1B(0.5) O14(0.5) O13(0.5) C1C(0.5) H1CA(0.5)
 H1CB(0.5) H1CC(0.5) C188(0.75) H188(0.75) O18(0.25) O17(0.25) C191(0.25)
 H19A(0.25) H19B(0.25) H19C(0.25) C1D(0.25) C1E(0.25) H1E(0.25) F3A(0.25)
 C0AA(0.75) H0AA(0.75) H0AB(0.75) H0AC(0.75) O19(0.75) C163(0.5) H163(0.5)
6.a Ternary CH refined with riding coordinates:
 C216(H216), C25(H25), C166(H166), C19(H19), C95(H95), C101(H101), C57(H57),
 C204(H204), C73(H73), C159(H159), C210(H210), C188(H188), C1E(H1E), C163(H163)
6.b Me refined with riding coordinates:
 C213(H21G,H21H,H21I), C191(H19A,H19B,H19C), C211(H21J,H21K,H21L), C0AA(H0AA,
 H0AB,H0AC)
6.c Aromatic/amide H refined with riding coordinates:
 C85(H85), C149(H149), C84(H84), C223(H223), C222(H222), C196(H196),
 C152(H152), C221(H221), C220(H220), C108(H108), C111(H111), C123(H123),
 C30(H30), C106(H106), C129(H129), C132(H132), C165(H165), C100(H100),
 C148(H148), C176(H176), C140(H140), C89(H89), C227(H227), C8(H8), C171(H171),
 C18(H18), C83(H83), C03I(H03I), C178(H178), C147(H147), C141(H141), C72(H72),
 C199(H199), C53(H53), C144(H144), C134(H134), C94(H94), C194(H194), C228(H228),
  C13(H13), C9(H9), C170(H170), C177(H177), C138(H138), C32(H32), C50(H50),
 C193(H193), C198(H198), C181(H181), C107(H107), C31(H31), C45(H45), C133(H133),
  C92(H92), C172(H172), C112(H112), C1(H1), C47(H47), C173(H173), C7(H7),
 C56(H56), C201(H201), C4(H4), C15(H15), C24(H24), C3(H3), C46(H46), C63(H63),
 C155(H155), C2(H2), C142(H142), C184(H184), C42(H42), C121(H121), C122(H122),
 C64(H64), C126(H126), C143(H143), C158(H158), C62(H62), C139(H139), C137(H137),
  C200(H200), C41(H41), C38(H38), C114(H114), C40(H40), C70(H70), C39(H39),
 C77(H77), C37(H37), C203(H203), C215(H215), C80(H80), C209(H209), C67(H67),
 C113(H113), C36(H36), C118(H118), C35(H35), C119(H119), C68(H68), C117(H117),
 C69(H69), C116(H116), C78(H78), C79(H79), C187(H187), C32A(H32A)
6.d Fitted pentagon refined as free rotating group:
 C186(N52,N53,N54,C187)
6.e Idealised Me refined as rotating group:
 C167(H16A,H16B,H16C), C26(H26A,H26B,H26C), C20(H20G,H20H,H20I), C169(H16D,
 H16E,H16F), C98(H98A,H98B,H98C), C102(H10A,H10B,H10C), C205(H20A,H20B,H20C),
 C96(H96A,H96B,H96C), C22(H22A,H22B,H22C), C28(H28A,H28B,H28C), C104(H10D,H10E,
 H10F), C76(H76A,H76B,H76C), C74(H74A,H74B,H74C), C60(H60A,H60B,H60C),
 C217(H21A,H21B,H21C), C207(H20D,H20E,H20F), C58(H58A,H58B,H58C), C160(H16G,
 H16H,H16I), C162(H16J,H16K,H16L), C219(H21D,H21E,H21F), C189(H18A,H18B,H18C),
 C1C(H1CA,H1CB,H1CC)
;
_shelx_res_checksum              71322
_shelx_fab_checksum              80135
_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
;