Construction of a chiral zinc–camphorate framework for enantioselective separation
Zhu, Chengfeng; Wang, Hongzhao; Mu, Yongfei; Zhang, Ziwei; Cheng, Lanjun; Li, Tianfu; Fu, Yanming; Wu, Xiang; Li, Yougui; Dalton Transactions  (2022) –; doi:10.1039/D2DT01221A

data_7710501
_publ_section_title
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 Construction of a chiral zinc--camphorate framework for enantioselective
 separation
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT01221A
_journal_year                    2022
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C38 H45 N4 O12 Zn2, 2[C3H7NO], 2[CH4O]'
_chemical_formula_sum            'C46 H67 N6 O16 Zn2'
_chemical_formula_weight         1090.79
_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_block_doi                 10.5517/ccdc.csd.cc2brcyf
_audit_creation_date             2022-05-06
_audit_creation_method
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Olex2 1.5-dev
(compiled 2022.05.04 svn.r4f934e98 for OlexSys, GUI svn.r6444)
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_audit_update_record
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2022-05-23 deposited with the CCDC.	2022-06-15 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 98.647(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.1892(13)
_cell_length_b                   20.317(3)
_cell_length_c                   17.675(3)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.837
_cell_measurement_theta_min      2.187
_cell_volume                     2907.3(8)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.67042
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_av_unetI/netI     0.0917
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30162
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        23.719
_diffrn_reflns_theta_max         23.927
_diffrn_reflns_theta_min         1.099
_exptl_absorpt_coefficient_mu    0.763
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.5437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1289 before and 0.0936 after correction.
The Ratio of minimum to maximum transmission is 0.7298.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             1146
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.38(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         10347
_refine_ls_number_restraints     489
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1134
_refine_ls_R_factor_gt           0.0879
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1751P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2480
_refine_ls_wR_factor_ref         0.2705
_reflns_Friedel_coverage         0.903
_reflns_Friedel_fraction_full    0.948
_reflns_Friedel_fraction_max     0.940
_reflns_number_gt                7428
_reflns_number_total             10347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01221a2.cif
_cod_data_source_block           sad
_cod_database_code               7710501
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.62(3)
 0.38(3)
2. 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, All O(H,H) groups
3. Rigid body (RIGU) restrains
 C27, O4, C7, Zn2, O3, C5, N1, O5, O11, O6, C8, C4, C6, C21, C25, C11, C2, C9,
 C10, C3, C22, C24, C12, C1, C23, C16, C13, O2, O1, N2, C15, C18, C17, C14, C26,
  C19, C20, O9, O7, O8, C32, C28, C31, C29, C30, C33, O10, N3, C34, C38, C35,
 C37, C36, N4, Zn1, O12
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Rotating group:
 O11(H11A,H11B), O12(H12A,H12B)
4.b Ternary CH refined with riding coordinates:
 C12(H12), C2(H2A)
4.c Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C3(H3A,H3B), C14(H14A,H14B)
4.d Aromatic/amide H refined with riding coordinates:
 N2(H2), C38(H38), C35(H35), C36(H36), C37(H37), C21(H21), C22(H22), C24(H24),
 C25(H25), N3(H3), C32(H32), C28(H28), C29(H29), C31(H31), C13(H13)
4.e Fitted hexagon refined as free rotating group:
 C38(C34,C35,C36,N4,C37), N1(C21,C22,C23,C24,C25), C32(C27,C28,C29,C30,C31)
4.f Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C17(H17A,H17B,H17C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C)
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_smtbx_masks_special_details
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A solvent mask was calculated and 232 electrons were 
found in a volume of 1166\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 2[C3H7NO], 2[CH4O] per Formula Unit 
which account for 232 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              98741
_shelx_fab_checksum              17621
_olex2_submission_special_instructions 'No special instructions were received'