Chiral Molecular Nanosilicas
Zong, Zhaohui; Hao, Aiyou; Xing, Pengyao; Zhao, Yanli; Chemical Science  (2022) –; doi:10.1039/D2SC00793B

data_1566608
_publ_section_title
;
 Chiral Molecular Nanosilicas
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00793B
_journal_year                    2022
_chemical_formula_moiety         'C84 H166 Fe N4 O28 Si16, 2(C4 H8 O2)'
_chemical_formula_sum            'C92 H182 Fe N4 O32 Si16'
_chemical_formula_weight         2361.70
_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   mixed
_audit_creation_date             2021-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-15 deposited with the CCDC.	2022-03-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.980(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.9205(5)
_cell_length_b                   17.5657(5)
_cell_length_c                   21.7093(5)
_cell_measurement_reflns_used    16049
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      76.2570
_cell_measurement_theta_min      3.1760
_cell_volume                     6451.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.938
_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      6.00  66.00   1.00    0.60    --   48.45 -70.00 -15.00   60
  2  \w     29.00  60.00   1.00    0.60    --   48.45  70.00 116.00   31
  3  \w    -68.00  14.00   1.00    0.60    --  -48.45  70.00 116.00   82
  4  \w   -120.00 -28.00   1.00    0.60    --  -48.45 -70.00 -15.00   92
  5  \w   -120.00 -73.00   1.00    0.60    --  -48.45-125.00 120.00   47
  6  \w    -65.00 -25.00   1.00    7.00    --  -86.25  70.00 116.00   40
  7  \w   -158.00-124.00   1.00    7.00    --  -86.25 -70.00 -15.00   34
  8  \w    101.00 138.00   1.00    7.00    --  106.49  38.00  60.00   37
  9  \w    141.00 178.00   1.00    7.00    --  106.49  38.00  60.00   37
 10  \w     87.00 168.00   1.00    7.00    --  106.49  70.00 116.00   81
 11  \w     58.00 105.00   1.00    7.00    --  106.49 -77.00  30.00   47
 12  \w     37.00 110.00   1.00    7.00    --  106.49-125.00   0.00   73
 13  \w     34.00  87.00   1.00    7.00    --  106.49 -70.00 -15.00   53
 14  \w     34.00  63.00   1.00    7.00    --  106.49 -57.00-120.00   29
 15  \w     35.00  66.00   1.00    7.00    --  106.49 -57.00-150.00   31
 16  \w     34.00 111.00   1.00    7.00    --  106.49-125.00 -30.00   77
 17  \w     92.00 178.00   1.00    7.00    --  106.49  57.00-150.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0669783000
_diffrn_orient_matrix_UB_12      0.0443916000
_diffrn_orient_matrix_UB_13      -0.0311511000
_diffrn_orient_matrix_UB_21      0.0063871000
_diffrn_orient_matrix_UB_22      0.0530681000
_diffrn_orient_matrix_UB_23      0.0562674000
_diffrn_orient_matrix_UB_31      0.0614328000
_diffrn_orient_matrix_UB_32      -0.0539056000
_diffrn_orient_matrix_UB_33      0.0299005000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39020
_diffrn_reflns_point_group_measured_fraction_full 0.820
_diffrn_reflns_point_group_measured_fraction_max 0.761
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.133
_diffrn_reflns_theta_min         2.612
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.924
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77580
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       block
_exptl_crystal_F_000             2536
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dioxane/Cyclohexane'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.164
_refine_ls_abs_structure_details
;
 Flack x determined using 5311 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.044(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1335
_refine_ls_number_reflns         20791
_refine_ls_number_restraints     459
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1169
_refine_ls_R_factor_gt           0.1084
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+15.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2987
_refine_ls_wR_factor_ref         0.3063
_reflns_Friedel_coverage         0.568
_reflns_Friedel_fraction_full    0.641
_reflns_Friedel_fraction_max     0.571
_reflns_number_gt                17658
_reflns_number_total             20791
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00793b2.cif
_cod_data_source_block           210305f
_cod_database_code               1566608
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         FeSiC
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.844
_diffrn_oxdiff_digest_frames
;
01e95374688dc0c79339588ba506d5682e00937aed6
;
_diffrn_oxdiff_digest_hkl
;
016d3b5574e92b1a09b27175bab28c02b29523
;
_reflns_odcompleteness_completeness 98.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C36-C35 = C10-C36 = C7-C36
 1.53 with sigma of 0.01
 C34-C33 = C34-C27 = C23-C34 = C48-C2 = C49-C48 = C48-C47 = C32-C1 = C32-C3 =
 C32-C31 = C51-C50 = C53-C51 = C52-C51 = C10-C36 = C7-C36 = C36-C35
 1.53 with sigma of 0.01
 C13-C54
 1.53 with sigma of 0.01
 C22-C62 = C19-C62 = C79-C6 = C9-C6 = C16-C30 = C16-C26 = C80-C16 = C21-C64 =
 C64-C24 = C64-C63 = C66-C8 = C66-C5 = C66-C65
 1.53 with sigma of 0.01
 C12-C67
 1.53 with sigma of 0.01
 C14-C12 = C17-C12
 1.53 with sigma of 0.01
 C20-C37 = C20-C28 = C20-C25
 1.53 with sigma of 0.01
 O31-C90 = O31-C92 = O32-C91 = O32-C93
 1.45 with sigma of 0.01
 C92-C91 = C93-C90
 1.51 with sigma of 0.01
 C86-O30
 1.45 with sigma of 0.01
 O30-C89 = O0AA-C87 = O0AA-C88
 1.45 with sigma of 0.01
 C93-C91
 2.2 with sigma of 0.02
 C92-C90
 2.2 with sigma of 0.02
 C15-C13 = C18-C13
 1.53 with sigma of 0.01
 C15-C18
 2.4 with sigma of 0.02
 C60-C6
 1.53 with sigma of 0.01
 C60-C9
 2.4 with sigma of 0.02
 C79-C60
 2.4 with sigma of 0.02
 H93A-H91B
 2.2 with sigma of 0.02
 H2A-H60A_$1
 2.2 with sigma of 0.02
 H86B-H89A
 2.2 with sigma of 0.02
 H60B-H79A
 2.2 with sigma of 0.02
 H2C-H60A_$1
 2.2 with sigma of 0.02
 H26B-H60C_$2
 2.2 with sigma of 0.02
3. Rigid bond restraints
 C12, C14, C17, C67
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O31, O32, C90, C91, C92, C93
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O0AA, O30, C86, C87, C88, C89
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C13, C15, C18, C54
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C9, C60, C79
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C27, C34, C23, C33
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C61 \\sim C62 \\sim C19 \\sim C22: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01
Si12 \\sim C6 \\sim C9 \\sim C60 \\sim C79: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.01
C16 \\sim C30 \\sim C26 \\sim C80: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C23) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C1)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C7) \\sim Ueq,
Uanis(C36) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C12) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C22)
\\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C16) \\sim Ueq,
Uanis(C26) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C24)
\\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C9) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C20) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C25) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O31) \\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C92) \\sim Ueq, Uanis(C93)
\\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(O32) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C89) \\sim Ueq, Uanis(O0AA) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(C88)
\\sim Ueq, Uanis(C86) \\sim Ueq, Uanis(O30) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C15) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C13) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C60) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Riding coordinates:
 C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C60(H60A,H60B,H60C)
5.b Ternary CH refined with riding coordinates:
 C6(H6), C12(H12), C13(H13), C16(H16), C20(H20), C32(H32), C34(H34), C36(H36),
 C42(H42), C44(H44), C48(H48), C51(H51), C62(H62), C64(H64), C66(H66), C72(H72),
  C74(H74), C78(H78)
5.c Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,
 H38B), C39(H39A,H39B), C40(H40A,H40B), C47(H47A,H47B), C50(H50A,H50B),
 C54(H54A,H54B), C61(H61A,H61B), C63(H63A,H63B), C65(H65A,H65B), C67(H67A,H67B),
  C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B), C77(H77A,H77B), C79(H79A,
 H79B), C80(H80A,H80B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B),
 C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B), C93(H93A,H93B)
5.d Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C56(H56), C57(H57), C58(H58), C59(H59),
 C82(H82), C83(H83), C84(H84), C85(H85)
5.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,
 H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,
 H10C), C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C17(H17A,H17B,H17C), C19(H19A,
 H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C),
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C45(H45A,H45B,H45C), C46(H46A,
 H46B,H46C), C49(H49A,H49B,H49C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C75(H75A,H75B,H75C), C76(H76A,H76B,H76C)
;
_shelx_res_checksum              52288
_shelx_hkl_checksum              24772
_shelx_fab_checksum              31327
_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 1.830
_oxdiff_exptl_absorpt_empirical_full_min 0.685