The crystal structure of methyl 5-nitro-2-(tosyloxy)benzoate, C15H13NO7S
Deng, Shao-Wen; Yuan, Lin; Li, Zhong-Yan; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 1133–1134; doi:10.1515/ncrs-2023-0360

data_8107682
_publ_section_title
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 The crystal structure of methyl 5-nitro-2-(tosyloxy)benzoate, C15H13NO7S
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1133
_journal_page_last               1134
_journal_paper_doi               10.1515/ncrs-2023-0360
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C15 H13 N O7 S'
_chemical_formula_sum            'C15 H13 N O7 S'
_chemical_formula_weight         351.32
_chemical_name_systematic
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methyl 5-nitro-2-(tosyloxy)benzoate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                79.1416(18)
_cell_angle_beta                 79.4782(16)
_cell_angle_gamma                81.1835(18)
_cell_formula_units_Z            2
_cell_length_a                   6.5990(11)
_cell_length_b                   7.7259(13)
_cell_length_c                   16.428(3)
_cell_measurement_reflns_used    5563
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      2.56
_cell_volume                     802.6(2)
_computing_cell_refinement       'Bruker SMART [1]'
_computing_data_collection       'Bruker SMART [1]'
_computing_data_reduction        'Bruker SAINT [1]'
_computing_molecular_graphics    'Bruker SHELXTL [1]'
_computing_publication_material  'Bruker SHELXTL [1]'
_computing_structure_refinement  'SHELXL, OLEX2 [3-4]'
_computing_structure_solution    'SHELXT  [2]'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0125
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7654
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         1.278
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.239
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6953
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0519 before and 0.0251 after correction.
The Ratio of minimum to maximum transmission is 0.9325.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_description       block
_exptl_crystal_F_000             364
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.035
_refine_ls_extinction_coef       0.034(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+0.2504P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0921
_refine_ls_wR_factor_ref         0.0960
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2548
_reflns_number_total             2813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0360_suppl_001.cif
_cod_data_source_block           0m
_cod_database_code               8107682
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C14(H14), C3(H3), C4(H4), C10(H10), C13(H13), C11(H11)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C8(H8A,H8B,H8C)
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_shelx_res_checksum              35951
_shelx_hkl_checksum              66951
_olex2_submission_special_instructions 'No special instructions were received'