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

data_1566609
_publ_section_title
;
 Chiral Molecular Nanosilicas
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC00793B
_journal_year                    2022
_chemical_formula_moiety
'0.5(C80 Fe N4 O27 S2 Si16), 0.5(C71 Fe N4 O28 S Si16), 0.5(C2 S)'
_chemical_formula_sum            'C76.5 Fe N4 O27.5 S2 Si16'
_chemical_formula_weight         1984.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_audit_creation_date             2021-07-11
_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                 103.053(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   37.4731(9)
_cell_length_b                   17.2234(3)
_cell_length_c                   42.6209(11)
_cell_measurement_reflns_used    16940
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      75.7820
_cell_measurement_theta_min      2.8180
_cell_volume                     26797.4(11)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.936
_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     34.00  65.00   1.00   18.00    --  106.49 -57.00  60.00   31
  2  \w     34.00  66.00   1.00   18.00    --  106.49 -57.00  90.00   32
  3  \w     34.00  66.00   1.00   18.00    --  106.49 -57.00 120.00   32
  4  \w    -10.00  36.00   1.00    1.60    --   48.32 -31.00  65.00   46
  5  \w     75.00 111.00   1.00   18.00    --  106.49-125.00 -60.00   36
  6  \w     36.00 105.00   1.00   18.00    --  106.49 -77.00 -90.00   69
  7  \w     95.00 176.00   1.00   18.00    --  106.49  19.00 -30.00   81
  8  \w    134.00 161.00   1.00   18.00    --  106.49  31.00-134.00   27
  9  \w     94.00 172.00   1.00   18.00    --  106.49  19.00-150.00   78
 10  \w     50.00  77.00   1.00    1.60    --   48.32  31.00-134.00   27
 11  \w     34.00  65.00   1.00   18.00    --  106.49 -57.00 -60.00   31
 12  \w     39.00  66.00   1.00   18.00    --  106.49 -57.00-150.00   27
 13  \w     35.00  72.00   1.00   18.00    --  106.49-125.00 -60.00   37
 14  \w    -35.00  26.00   1.00    1.60    --  -48.32  31.00-134.00   61
 15  \w    -27.00  27.00   1.00    1.60    --  -48.32  19.00  30.00   54
 16  \w    -66.00 -14.00   1.00   18.00    --  -86.25  57.00  30.00   52
 17  \w   -122.00 -37.00   1.00    1.60    --  -48.32 -31.00  65.00   85
 18  \w   -141.00-116.00   1.00   18.00    --  -86.25 -31.00  65.00   25
 19  \w   -142.00 -71.00   1.00   18.00    --  -86.25 -57.00  90.00   71
;
_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      -0.0383057000
_diffrn_orient_matrix_UB_12      -0.0299503000
_diffrn_orient_matrix_UB_13      -0.0169625000
_diffrn_orient_matrix_UB_21      0.0078632000
_diffrn_orient_matrix_UB_22      0.0206979000
_diffrn_orient_matrix_UB_23      -0.0329323000
_diffrn_orient_matrix_UB_31      0.0159691000
_diffrn_orient_matrix_UB_32      -0.0816944000
_diffrn_orient_matrix_UB_33      -0.0020843000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0662
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            81724
_diffrn_reflns_point_group_measured_fraction_full 0.762
_diffrn_reflns_point_group_measured_fraction_max 0.708
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         26.596
_diffrn_reflns_theta_min         1.307
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.339
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82487
_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_density_diffrn    0.984
_exptl_crystal_F_000             7912
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM/MeOH'
_refine_diff_density_max         2.774
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.219
_refine_ls_abs_structure_details
;
 Flack x determined using 7372 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -1.155(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.778
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1860
_refine_ls_number_reflns         39871
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      1.801
_refine_ls_R_factor_all          0.1897
_refine_ls_R_factor_gt           0.1686
_refine_ls_shift/su_max          4.352
_refine_ls_shift/su_mean         0.349
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4223
_refine_ls_wR_factor_ref         0.4445
_reflns_Friedel_coverage         0.463
_reflns_Friedel_fraction_full    0.525
_reflns_Friedel_fraction_max     0.464
_reflns_number_gt                29814
_reflns_number_total             39871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc00793b2.cif
_cod_data_source_block           210118d
_cod_original_formula_sum        'C76.50 Fe N4 O27.50 S2 Si16'
_cod_database_code               1566609
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         FeCSi
_diffrn_oxdiff_digest_frames
;
014ff4e899ee2cbedb4efa0cdb1f359fa500902e782
;
_diffrn_oxdiff_digest_hkl
;
013c3f5350b9ab8386fe5ba2d8f75e2f89b67e
;
_reflns_odcompleteness_completeness 98.52
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Restrained distances
 Si-O03S
 1.55 with sigma of 0.01
 Si4-O01Z
 1.55 with sigma of 0.01
 O24-Si0T
 1.55 with sigma of 0.01
 O03S-Si2
 1.55 with sigma of 0.01
 O04R-Si0U
 1.55 with sigma of 0.01
 Si-O68
 1.55 with sigma of 0.01
 O04P-Si
 1.55 with sigma of 0.01
 O68-Si3
 1.55 with sigma of 0.01
 O04R-Si3
 1.55 with sigma of 0.01
 O03Q-Si01
 1.55 with sigma of 0.01
 Si1-O03Q
 1.55 with sigma of 0.01
 C04X-C03R = C04H-C03R = C03R-C033 = C04A-C037 = C05O-C04A = C059-C04A = C031-
 C030 = C050-C030 = C04O-C030 = C05R-C04N = C061-C04N = C04N-C02Z = C05T-C040 =
 C040-C03T = C05I-C040 = C80-C03D = C80-C67 = C80-C27 = C04I-C03Y = C067-C04I =
 C05U-C04I
 1.53 with sigma of 0.01
 Si3-O68 = Si-O68 = Si-O04P = Si0T-O04P = Si0T-O02M = Si0T-O24 = Si4-O24 = Si4-
 O06E = Si3-O06E = Si1-O01Z = Si4-O01Z = Si1-O05G = Si0U-O05G = Si0U-O035 = Si2-
 O035 = Si2-O03S = Si2-O06K = Si01-O06K = Si01-O03Q = Si1-O03Q = Si0U-O04R =
 Si3-O04R = Si01-O02M = Si-O03S
 1.59 with sigma of 0.01
 C070-C060
 1.53 with sigma of 0.01
 C07G-C070
 1.53 with sigma of 0.01
 C04G-C04F = C112-C04G = C04G-C043 = C052-C034 = C056-C034
 1.53 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(Si3) \\sim Ueq, Uanis(Si4) \\sim Ueq, Uanis(Si0T) \\sim Ueq, Uanis(Si)
\\sim Ueq, Uanis(Si2) \\sim Ueq, Uanis(Si01) \\sim Ueq, Uanis(Si0U) \\sim Ueq,
Uanis(Si1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Sof(S2)=Sof(C2)=Sof(C46)=1-FVAR(1)
 Sof(S5)=Sof(C222)=Sof(C28)=FVAR(1)
;
_shelx_res_checksum              6792
_shelx_hkl_checksum              9803
_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 1.485
_oxdiff_exptl_absorpt_empirical_full_min 0.711