Enantiopure chiroptical probes for circular dichroism and absorbance based detection of nerve gas simulants.
Debnath, Snehasish; Chatterjee, Pabitra B.; Chemical communications (Cambridge, England) 58 (2022) 9006–9009; doi:10.1039/d2cc03392e

data_7130651
_publ_section_title
;
 Enantiopure chiroptical probes for circular dichroism and absorbance
 based detection of nerve gas simulants.
;
_journal_issue                   64
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9006
_journal_page_last               9009
_journal_paper_doi               10.1039/d2cc03392e
_journal_volume                  58
_journal_year                    2022
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C21 H29 N O3, 1/3(H2 O)'
_chemical_formula_sum            'C21 H29.66667 N O3.33333'
_chemical_formula_weight         349.46
_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             2022-06-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-06-15 deposited with the CCDC.	2022-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.6730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   10.8179(2)
_cell_length_b                   20.9974(5)
_cell_length_c                   13.8796(2)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      33.47
_cell_measurement_theta_min      2.26
_cell_volume                     2909.08(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0452
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23464
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.94
_diffrn_source                   'MICRO FOCUS TUBE'
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.6987
_exptl_absorpt_correction_T_min  0.5926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.197
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         9607
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0394
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+0.5371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0881
_refine_ls_wR_factor_ref         0.0902
_reflns_number_gt                9057
_reflns_number_total             9607
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc03392e5.cif
_cod_data_source_block           SND406ligand2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

2024-12-16
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C63 H89 N3 O10'
_cod_original_formula_weight         1048.37
_cod_original_formula_moiety         '3(C21 H29 N O3), H2 O'
_cod_original_formula_units_Z            2
_cod_database_code               7130651
_olex2_refinement_description
;
1. Restrained distances
 H2O-O10 = H1O-O10
 0.82 with sigma of 0.02
2.a Ternary CH refined with riding coordinates:
 C10(H10), C31(H31), C52(H52)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C12(H12A,H12B), C13(H13A,H13B), C30(H30A,H30B), C33(H33A,H33B),
 C34(H34A,H34B), C51(H51A,H51B), C54(H54A,H54B), C55(H55A,H55B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C17(H17), C19(H19), C25(H25), C27(H27), C38(H38), C40(H40),
 C46(H46), C48(H48), C59(H59), C61(H61)
2.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C),
 C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C32(H32A,H32B,
 H32C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C53(H53A,H53B,H53C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C)
2.e Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3), O4(H4A), O5(H5), O6(H6A), O7(H7), O8(H8), O9(H9)
;
_shelx_res_checksum              42551
_shelx_hkl_checksum              7814
_olex2_submission_special_instructions 'No special instructions were received'