Polymorphism and molecular conformations of nicosulfuron: structure, properties and desolvation process
Liu, Yu; Jia, Lina; Wu, Songgu; Xu, Shijie; Zhang, Xu; Jiang, Shuang; Gong, Junbo; CrystEngComm 21 (2019) 2790–; doi:10.1039/C8CE02074D

data_7232536
_publ_section_title
;
 Polymorphism and molecular conformations of nicosulfuron: structure,
 properties and desolvation process
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              2790
_journal_paper_doi               10.1039/C8CE02074D
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C15 H18 N6 O6 S, C H4 O'
_chemical_formula_sum            'C16 H22 N6 O7 S'
_chemical_formula_weight         442.45
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2018-12-03 deposited with the CCDC.    2019-03-22 downloaded from the CCDC.
;
_cell_angle_alpha                85.55(3)
_cell_angle_beta                 83.76(3)
_cell_angle_gamma                85.07(3)
_cell_formula_units_Z            8
_cell_length_a                   7.8533(16)
_cell_length_b                   20.401(4)
_cell_length_c                   25.859(5)
_cell_measurement_reflns_used    7497
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9304
_cell_measurement_theta_min      1.3225
_cell_volume                     4093.5(14)
_computing_cell_refinement       crystalclear
_computing_data_collection       crystalclear
_computing_data_reduction        crystalclear
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku Saturn 70'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0877
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            47780
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.904
_diffrn_reflns_theta_min         1.322
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.210
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       prism
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0030(4)
_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   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1106
_refine_ls_number_reflns         19378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1316
_refine_ls_R_factor_gt           0.0684
_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^)+(0.0789P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1946
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10031
_reflns_number_total             19378
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce02074d2.cif
_cod_data_source_block           shelxl_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7232534--7232536.cif.'
_cod_original_cell_volume        4093.5(15)
_cod_database_code               7232536
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4B(H4B), N3B(H3B), C10B(H10B), C11B(H11B), C12B(H12B), C3B(H3BA), N4C(H4C),
 N3C(H3C), C10C(H10C), C11C(H11C), C12C(H12C), C3C(H3CA), N4D(H4D), N3D(H3D),
 C10D(H10D), C11D(H11D), C12D(H12D), C3D(H3DA), N4A(H4A), N3A(H3A), C10A(H10A),
 C11A(H11A), C12A(H12A), C3A(H3AA)
2.b Idealised Me refined as rotating group:
 C15B(H15A,H15B,H15C), C14B(H14A,H14B,H14C), C5B(H5BA,H5BB,H5BC), C6B(H6BA,
 H6BB,H6BC), C15C(H15D,H15E,H15F), C14C(H14D,H14E,H14F), C6C(H6CA,H6CB,H6CC),
 C5C(H5CA,H5CB,H5CC), C15D(H15G,H15H,H15I), C14D(H14G,H14H,H14I), C5D(H5DA,H5DB,
 H5DC), C6D(H6DA,H6DB,H6DC), C14A(H14J,H14K,H14L), C15A(H15J,H15K,H15L),
 C6A(H6AA,H6AB,H6AC), C5A(H5AA,H5AB,H5AC), C0AA(H0AB,H0AC,H0AD), C3S(H3SA,H3SB,
 H3SC), C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC)
2.c Idealised tetrahedral OH refined as rotating group:
 O0AA(H0AA), O3S(H3S), O1S(H1S), O2S(H2S)
;
_shelx_res_checksum              13829
_olex2_submission_special_instructions 'No special instructions were received'