A novel pyrazolium ionic liquid used for CO2 cycloaddition
Li, Jun-Fei; Guan, Xiao-Hui; Feng, Hui-Jun; Zhou, Dai-Mei; Liu, Qiao-Yun; Zhang, Wen-Yao; Guo, Cai-Hong; Bai, Jun-Hua; Wang, Jun-Wen; New Journal of Chemistry 48 (2024) 12706–12712; doi:10.1039/D4NJ01776E

data_7063282
_publ_section_title
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 A novel pyrazolium ionic liquid used for CO2 cycloaddition
;
_journal_issue                   28
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12706
_journal_page_last               12712
_journal_paper_doi               10.1039/D4NJ01776E
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C19 H21 N2, Br, H2 O'
_chemical_formula_sum            'C19 H23 Br N2 O'
_chemical_formula_weight         375.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2023-12-25
_audit_creation_method
; 
Olex2 1.5 
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) 
;
_audit_update_record
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2024-02-20 deposited with the CCDC.	2024-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.492(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.9502(13)
_cell_length_b                   10.2847(9)
_cell_length_c                   24.072(2)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      65.12
_cell_measurement_theta_min      3.72
_cell_volume                     3650.6(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            32836
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        65.384
_diffrn_reflns_theta_max         65.384
_diffrn_reflns_theta_min         2.997
_diffrn_source_current           1.2
_diffrn_source_power             0.06
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.106
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. 
wR2(int) was 0.1197 before and 0.0608 after correction. 
The Ratio of minimum to maximum transmission is 0.8394. 
The \l/2 correction factor is Not present. 
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.734
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     419
_refine_ls_number_reflns         6184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0595P)^2^+3.5083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1183
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5219
_reflns_number_total             6184
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj01776e2.cif
_cod_data_source_block           cu_230826a_0m_a
_cod_depositor_comments          'Adding full bibliography for 7063282.cif.'
_cod_original_cell_volume        3650.6(6)
_cod_database_code               7063282
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.746
_shelx_estimated_absorpt_t_min   0.707
_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,H) groups 
2.a Riding coordinates: 
 O1(H1A,H1B), O2(H2A,H2B) 
2.b Secondary CH2 refined with riding coordinates: 
 C26(H26A,H26B), C33(H33A,H33B), C7(H7A,H7B), C13(H13A,H13B) 
2.c Aromatic/amide H refined with riding coordinates: 
 C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C28(H28), C29(H29), 
 C30(H30), C31(H31), C32(H32), C35(H35), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), 
  C9(H9), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19) 
2.d Idealised Me refined as rotating group: 
 C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C11(H11A,H11B,H11C), C12(H12A,H12B, 
 H12C) 
;
_shelx_res_checksum              87234
_shelx_hkl_checksum              31790
_olex2_submission_special_instructions 'No special instructions were received'