Assemblies of salts of urea and thiourea derivatives and release of hosts from composites with calcium oxide
Brahma, Rinki; Baruah, Jubaraj Bikash; New Journal of Chemistry 47 (2023) 6211–6223; doi:10.1039/D2NJ05412D

data_7062313
_publ_section_title
;
 Assemblies of salts of urea and thiourea derivatives and release of hosts
 from composites with calcium oxide
;
_journal_issue                   13
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              6211
_journal_page_last               6223
_journal_paper_doi               10.1039/D2NJ05412D
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C17 H16 N3 O, Cl O4, H2 O'
_chemical_formula_sum            'C17 H18 Cl N3 O6'
_chemical_formula_weight         395.79
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2023-02-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-22 deposited with the CCDC.	2023-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.990(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.886(3)
_cell_length_b                   8.2613(18)
_cell_length_c                   20.140(5)
_cell_measurement_reflns_used    9517
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.53
_cell_measurement_theta_min      2.56
_cell_volume                     1789.0(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0597
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25145
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.046
_diffrn_reflns_theta_max         25.046
_diffrn_reflns_theta_min         2.563
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1709 before and 0.1056 after correction.
The Ratio of minimum to maximum transmission is 0.8118.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.6051
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3124
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0877P)^2^+2.1745P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1860
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2554
_reflns_number_total             3124
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj05412d3.cif
_cod_data_source_block           HnaphureaClO4H2O
_cod_depositor_comments
'Adding full bibliography for 7062311--7062319.cif.'
_cod_original_cell_volume        1789.0(7)
_cod_database_code               7062313
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Cl1-O5 \\sim Cl1-O5A
 with sigma of 0.02
 Cl1-O4 \\sim Cl1-O4A
 with sigma of 0.02
 Cl1-O2 \\sim Cl1-O2A
 with sigma of 0.02
 Cl1-O3 \\sim Cl1-O3A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3A) = Uanis(O3)
Uanis(O5A) = Uanis(O5)
Uanis(O2) = Uanis(O2A)
Uanis(O4A) = Uanis(O4)
4. Others
 Sof(O3A)=Sof(O5A)=Sof(O2A)=Sof(O4A)=1-FVAR(1)
 Sof(O5)=Sof(O4)=Sof(O2)=Sof(O3)=FVAR(1)
5.a Free rotating group:
 O6(H6A,H6B)
5.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
5.c Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), C2(H2A), C3(H3A), C7(H7), C10(H10), C17(H17),
 C14(H14), C15(H15), C9(H9), C8(H8), C4(H4), C16(H16)
;
_shelx_res_checksum              5430
_olex2_submission_special_instructions 'No special instructions were received'