#------------------------------------------------------------------------------
#$Date: 2020-11-06 14:47:20 +0200 (Fri, 06 Nov 2020) $
#$Revision: 258917 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/99/7059989.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7059989
loop_
_publ_author_name
'Nandi, Sujay Kumar'
'Haldar, Debasish'
_publ_section_title
;
 1-m-Nitrobenzoyl semicarbazide: reversible colorimetric cascade
 indicators for fluoride and moisture
;
_journal_issue                   40
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17523
_journal_page_last               17530
_journal_paper_doi               10.1039/D0NJ03769A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C8 H8 N4 O4'
_chemical_formula_sum            'C8 H8 N4 O4'
_chemical_formula_weight         224.18
_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
_audit_creation_date             2018-05-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_audit_update_record
;
2020-02-26 deposited with the CCDC.	2020-09-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.213(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.3611(5)
_cell_length_b                   4.6432(4)
_cell_length_c                   30.859(2)
_cell_measurement_reflns_used    5002
_cell_measurement_temperature    107(2)
_cell_measurement_theta_max      33.23
_cell_measurement_theta_min      2.65
_cell_volume                     908.98(12)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      107.49
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.876
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.876
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            12059
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.876
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.547
_diffrn_reflns_theta_min         2.647
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.134
_exptl_absorpt_correction_T_max  0.7468
_exptl_absorpt_correction_T_min  0.5559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_description       neddle
_exptl_crystal_F_000             464.0
_exptl_crystal_size_max          0.2358
_exptl_crystal_size_mid          0.2158
_exptl_crystal_size_min          0.1898
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         3397
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0877
_refine_ls_R_factor_gt           0.0593
_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/[σ²(Fo²)+(0.0645P)²+0.8176P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1406
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2509
_reflns_number_total             3397
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nj03769a2.cif
_cod_data_source_block           msc
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'multi scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7059989.cif.
;
_cod_original_cell_volume        908.97(13)
_cod_database_code               7059989
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
2.a Rotating group:
 N4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), C1(H1), C3(H3A), C5(H5), C4(H4)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O3 O 0.09198(19) 0.6680(3) 0.59128(4) 0.0202(3) Uani 1 1 d . . . . .
O4 O 0.25706(19) 0.4256(2) 0.48847(4) 0.0188(2) Uani 1 1 d . . . . .
O2 O 0.1403(2) -0.1181(3) 0.69691(4) 0.0239(3) Uani 1 1 d . . . . .
O1 O 0.4236(2) -0.1709(3) 0.73962(4) 0.0277(3) Uani 1 1 d . . . . .
N2 N 0.3907(2) 0.7506(3) 0.55721(4) 0.0184(3) Uani 1 1 d . . . . .
H2 H 0.5293 0.7454 0.5588 0.022 Uiso 1 1 calc R . . . .
N1 N 0.3230(2) -0.0573(3) 0.70880(5) 0.0186(3) Uani 1 1 d . . . . .
N4 N 0.1522(2) 0.8239(3) 0.44996(5) 0.0189(3) Uani 1 1 d . . . . .
H4A H 0.0663 0.7072 0.4347 0.023 Uiso 1 1 d GR . . . .
H4B H 0.0825 0.9792 0.4569 0.023 Uiso 1 1 d GR . . . .
N3 N 0.2796(2) 0.8656(3) 0.52111(4) 0.0190(3) Uani 1 1 d . . . . .
H3 H 0.2424 1.0482 0.5204 0.023 Uiso 1 1 calc R . . . .
C8 C 0.2289(2) 0.6897(3) 0.48657(5) 0.0158(3) Uani 1 1 d . . . . .
C2 C 0.4292(3) 0.1635(3) 0.68428(5) 0.0164(3) Uani 1 1 d . . . . .
C7 C 0.2835(2) 0.6458(3) 0.59014(5) 0.0161(3) Uani 1 1 d . . . . .
C6 C 0.4152(2) 0.5014(3) 0.62591(5) 0.0162(3) Uani 1 1 d . . . . .
C1 C 0.3153(2) 0.2954(3) 0.64999(5) 0.0160(3) Uani 1 1 d . . . . .
H1 H 0.1718 0.2466 0.6430 0.019 Uiso 1 1 calc R . . . .
C3 C 0.6376(3) 0.2312(4) 0.69622(5) 0.0202(3) Uani 1 1 d . . . . .
H3A H 0.7115 0.1387 0.7202 0.024 Uiso 1 1 calc R . . . .
C5 C 0.6260(3) 0.5712(4) 0.63700(5) 0.0187(3) Uani 1 1 d . . . . .
H5 H 0.6948 0.7103 0.6204 0.022 Uiso 1 1 calc R . . . .
C4 C 0.7356(3) 0.4381(4) 0.67218(6) 0.0214(3) Uani 1 1 d . . . . .
H4 H 0.8782 0.4890 0.6798 0.026 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N3 N2 H2 120.4 . . ?
C7 N2 H2 120.4 . . ?
C7 N2 N3 119.18(14) . . ?
O2 N1 C2 117.94(14) . . ?
O1 N1 O2 124.22(15) . . ?
O1 N1 C2 117.84(14) . . ?
H4A N4 H4B 109.3 . . ?
C8 N4 H4A 109.6 . . ?
C8 N4 H4B 109.3 . . ?
N2 N3 H3 120.8 . . ?
C8 N3 N2 118.44(13) . . ?
C8 N3 H3 120.8 . . ?
O4 C8 N4 122.56(15) . . ?
O4 C8 N3 122.07(15) . . ?
N4 C8 N3 115.34(14) . . ?
C1 C2 N1 118.00(14) . . ?
C1 C2 C3 122.75(15) . . ?
C3 C2 N1 119.25(14) . . ?
O3 C7 N2 123.17(15) . . ?
O3 C7 C6 121.40(14) . . ?
N2 C7 C6 115.43(14) . . ?
C1 C6 C7 116.70(14) . . ?
C1 C6 C5 119.71(15) . . ?
C5 C6 C7 123.53(15) . . ?
C2 C1 C6 118.64(15) . . ?
C2 C1 H1 120.7 . . ?
C6 C1 H1 120.7 . . ?
C2 C3 H3A 120.9 . . ?
C2 C3 C4 118.21(15) . . ?
C4 C3 H3A 120.9 . . ?
C6 C5 H5 119.8 . . ?
C4 C5 C6 120.32(15) . . ?
C4 C5 H5 119.8 . . ?
C3 C4 C5 120.36(16) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O3 C7 1.226(2) . ?
O4 C8 1.2398(19) . ?
O2 N1 1.2257(19) . ?
O1 N1 1.2257(19) . ?
N2 H2 0.8800 . ?
N2 N3 1.3823(19) . ?
N2 C7 1.355(2) . ?
N1 C2 1.468(2) . ?
N4 H4A 0.8815 . ?
N4 H4B 0.8818 . ?
N4 C8 1.350(2) . ?
N3 H3 0.8800 . ?
N3 C8 1.363(2) . ?
C2 C1 1.381(2) . ?
C2 C3 1.386(2) . ?
C7 C6 1.495(2) . ?
C6 C1 1.393(2) . ?
C6 C5 1.397(2) . ?
C1 H1 0.9500 . ?
C3 H3A 0.9500 . ?
C3 C4 1.389(2) . ?
C5 H5 0.9500 . ?
C5 C4 1.391(2) . ?
C4 H4 0.9500 . ?
