Synthesis and structural characterization of CO2-soluble oxidizers [Bu4N]BrO3 and [Bu4N]ClO3 and their dissolution in cosolvent-modified CO2 for reservoir applications
Hull, Katherine L.; Schipper, Desmond E.; Oliver, Allen G.; RSC Advances 10 (2020) 44973–44980; doi:10.1039/D0RA09563J

data_7241937
_publ_section_title
;
 Synthesis and structural characterization of CO2-soluble oxidizers
 [Bu4N]BrO3 and [Bu4N]ClO3 and their dissolution in cosolvent-modified CO2
 for reservoir applications
;
_journal_issue                   73
_journal_name_full               'RSC Advances'
_journal_page_first              44973
_journal_page_last               44980
_journal_paper_doi               10.1039/D0RA09563J
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C16 H36 N, Br O3, H2 O'
_chemical_formula_sum            'C16 H38 Br N O4'
_chemical_formula_weight         388.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-10-20 deposited with the CCDC.	2020-12-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.0239(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8000(4)
_cell_length_b                   12.7411(5)
_cell_length_c                   16.7622(6)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.76
_cell_volume                     2061.03(14)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 7.41
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker PHOTON-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0201
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            40837
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
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_diffrn_reflns_theta_max         28.273
_diffrn_reflns_theta_min         2.019
_diffrn_source                   'fine-focus sealed tube'
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_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6902
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Krause et al., 2015)'
_exptl_crystal_colour            colorless
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_exptl_crystal_description       block
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_exptl_crystal_size_max          0.343
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_exptl_crystal_size_min          0.134
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0244
_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^)+(0.0217P)^2^+1.1549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0538
_refine_ls_wR_factor_ref         0.0571
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4386
_reflns_number_total             5101
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra09563j2.cif
_cod_data_source_block           cmpd1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7241937
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.546
_shelx_estimated_absorpt_t_max   0.774
_diffrn_source_monochromator     'Bruker TRIUMPH curved-graphite'
_shelx_res_checksum              67353