Programming heterometallic 4f-4f' helicates under thermodynamic control: the circle is complete.
Egger, Charlotte; Guénée, Laure; Deorukhkar, Neel; Piguet, Claude; Dalton transactions (Cambridge, England : 2003) 53 (2024) 6050–6062; doi:10.1039/d4dt00610k

data_7715330
_publ_section_title
;
 Programming heterometallic 4f-4f' helicates under thermodynamic control:
 the circle is complete.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6050
_journal_page_last               6062
_journal_paper_doi               10.1039/d4dt00610k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C55 H50 N12 O, 2(C1.5 H4 O0.5)'
_chemical_formula_sum            'C58 H58 N12 O2'
_chemical_formula_weight         955.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-11-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-12-20 deposited with the CCDC.	2024-03-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.0349(17)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.7381(5)
_cell_length_b                   6.47585(9)
_cell_length_c                   42.6340(7)
_cell_measurement_reflns_used    13657
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      73.2840
_cell_measurement_theta_min      2.4600
_cell_volume                     9907.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.89a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.978
_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     35.00  63.00   0.50    1.00    --   64.07  15.00  90.00   56
  2  \w     51.00 121.00   0.50    1.00    --   77.28  15.00  90.00  140
  3  \w     59.00 116.00   0.50    1.00    --   77.28  15.00   0.00  114
  4  \w     37.00  63.00   0.50    1.00    --   72.58   0.00   0.00   52
  5  \w     33.00 109.00   0.50    1.00    --   64.07  15.00 -30.00  152
  6  \w     46.00  90.00   0.50    1.00    --   77.28  15.00 -90.00   88
  7  \w     49.00  96.00   0.50    1.00    --   77.28  15.00-180.00   94
  8  \w    -49.00 -21.00   0.50    1.00    --  -54.55   0.00-150.00   56
  9  \w    -91.00 -63.00   0.50    1.00    --  -54.55 -15.00 -30.00   56
 10  \w    -48.00 -23.00   0.50    1.00    --  -54.55 -15.00 -30.00   50
 11  \w     43.00  93.00   0.50    1.00    --   64.07-125.00 -60.00  100
 12  \w     40.00  98.00   0.50    1.00    --   77.28-125.00 -60.00  116
 13  \w     30.00  56.00   0.50    1.00    --   64.07 -94.00  30.00   52
 14  \w     28.00  63.00   0.50    1.00    --   64.07 -94.00 -30.00   70
 15  \w     40.00  77.00   0.50    1.00    --   77.28 -94.00 -30.00   74
 16  \w     52.00  98.00   0.50    1.00    --   72.58-125.00  90.00   92
 17  \w     80.00 106.00   0.50    1.00    --   77.28-125.00 150.00   52
 18  \w     48.00  85.00   0.50    1.00    --   77.28 -94.00 150.00   74
 19  \w     32.00  58.00   0.50    1.00    --   64.07 -94.00 150.00   52
 20  \w     40.00  65.00   0.50    1.00    --   77.28 -94.00  90.00   50
 21  \w     40.00  65.00   0.50    1.00    --   77.28 -94.00  60.00   50
 22  \w     27.00  56.00   0.50    1.00    --   64.07 -94.00  90.00   58
 23  \w     40.00  72.00   0.50    1.00    --   77.28 -94.00  30.00   64
 24  \w     45.00  70.00   0.50    1.00    --   77.28 -94.00   0.00   50
 25  \w     58.00  85.00   0.50    1.00    --   77.28 -94.00 -60.00   54
 26  \w     46.00  77.00   0.50    1.00    --   77.28 -94.00-120.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix-Arc 150'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0284880000
_diffrn_orient_matrix_UB_12      -0.1733294000
_diffrn_orient_matrix_UB_13      0.0016739000
_diffrn_orient_matrix_UB_21      -0.0143570000
_diffrn_orient_matrix_UB_22      -0.0203107000
_diffrn_orient_matrix_UB_23      -0.0378548000
_diffrn_orient_matrix_UB_31      0.0287230000
_diffrn_orient_matrix_UB_32      0.1617108000
_diffrn_orient_matrix_UB_33      -0.0029728000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_unetI/netI     0.0342
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            40064
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.254
_diffrn_reflns_theta_min         2.463
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  0.977
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.89a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
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    1.281
_exptl_crystal_description       plate
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         9853
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0758
_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^)+(0.0914P)^2^+22.8511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2031
_refine_ls_wR_factor_ref         0.2156
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7645
_reflns_number_total             9853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00610k2.cif
_cod_data_source_block           L4
_cod_depositor_comments
'Adding full bibliography for 7715330--7715332.cif.'
_cod_original_cell_volume        9907.2(3)
_cod_database_code               7715330
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C58 H58 N12 O2'
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.888
_reflns_odcompleteness_completeness 99.20
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_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, All O(H) groups
2. Restrained distances
 C4S-C2S = C2S-C3S
 1.54 with sigma of 0.02
 C58-C56A = C58-C57A
 1.54 with sigma of 0.02
 C58-C57B = C58-C56B
 1.54 with sigma of 0.02
 O3A-C58
 1.3 with sigma of 0.02
 O3B-C58
 1.3 with sigma of 0.02
 O1S-C2S
 1.3 with sigma of 0.02
 C56A-O3A
 2.3 with sigma of 0.04
 O3A-C57A
 2.3 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uiso(C3S) = Uiso(C4S)
Uiso(C56A) = Uiso(C57B) = Uiso(C57A) = Uiso(O3B) = Uiso(O3A) = Uiso(C56B)
4. Others
 Fixed Sof: H58A(0.25) H58(0.25) C56A(0.25) H56A(0.25) H56B(0.25) H56C(0.25)
 O3A(0.25) H3AA(0.25) C57A(0.25) H57A(0.25) H57B(0.25) H57C(0.25) C56B(0.25)
 H56D(0.25) H56E(0.25) H56F(0.25) O3B(0.25) H3BA(0.25) C57B(0.25) H57D(0.25)
 H57E(0.25) H57F(0.25) O1S(0.5) H1S(0.5) C2S(0.5) H2S(0.5) C4S(0.5) H4SA(0.5)
 H4SB(0.5) H4SC(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5) H3SC(0.5)
5.a Everything fixed:
 H3AA, H3BA, H1S
5.b Riding coordinates:
 C56A(H56A,H56B,H56C), C57A(H57A,H57B,H57C), C56B(H56D,H56E,H56F), C57B(H57D,
 H57E,H57F), C4S(H4SA,H4SB,H4SC), C3S(H3SA,H3SB,H3SC)
5.c Ternary CH refined with riding coordinates:
 C58(H58A), C58(H58), C2S(H2S)
5.d Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C19(H19A,H19B), C41(H41A,H41B)
5.e Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C14(H14), C15(H15), C17(H17), C21(H21), C22(H22),
 C25(H25), C29(H29), C30(H30), C31(H31), C36(H36), C37(H37), C39(H39), C43(H43),
  C48(H48), C49(H49), C51(H51), C52(H52), C54(H54)
5.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C12(H12A,H12B,H12C), C27(H27A,H27B,H27C),
 C34(H34A,H34B,H34C), C46(H46A,H46B,H46C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              92513
_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 1.537
_oxdiff_exptl_absorpt_empirical_full_min 0.655