Magnetic ordering in a vanadium-organic coordination polymer using a pyrrolo[2,3-d:5,4-d′]bis(thiazole)-based ligand
Getmanenko, Yulia A.; Mullins, Christopher S.; Nesterov, Vladimir N.; Lake, Stephanie; Risko, Chad; Johnston-Halperin, Ezekiel; RSC Advances 8 (2018) 36223–; doi:10.1039/C8RA05697H

data_7231691
_publ_section_title
;
 Magnetic ordering in a vanadium-organic coordination polymer using a
 pyrrolo[2,3-d:5,4-d&#x2032;]bis(thiazole)-based ligand
;
_journal_issue                   63
_journal_name_full               'RSC Advances'
_journal_page_first              36223
_journal_paper_doi               10.1039/C8RA05697H
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C12 H13 I2 N3 S2'
_chemical_formula_sum            'C12 H13 I2 N3 S2'
_chemical_formula_weight         517.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-09-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-17 deposited with the CCDC.
2018-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.6500(10)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   16.8767(2)
_cell_length_b                   33.8581(5)
_cell_length_c                   4.41650(10)
_cell_measurement_reflns_used    41565
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.1450
_cell_measurement_theta_min      2.1560
_cell_volume                     2522.60(7)
_computing_cell_refinement       'CrysAlisPro 1.171.40.12b (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.12b (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.12b (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -20.00  63.00   0.50   30.00    --   -5.49  39.00  10.61  166
  2  \w     21.00  61.00   0.50   30.00    --   -5.49  33.00  45.33   80
  3  \w     43.00  69.00   0.50   30.00    --   -5.49  33.00 142.30   52
  4  \w    -18.00  39.00   0.50   30.00    --    4.56 -99.00  30.00  114
  5  \w     18.00  43.00   0.50   30.00    --    4.56-106.00 -58.00   50
  6  \w    -19.00  62.00   0.50   30.00    --   -5.49  19.00 -90.00  162
  7  \w     39.00  65.00   0.50   30.00    --   -5.49  40.00-143.04   52
  8  \w    -20.00  21.00   0.50   30.00    --   -5.49  40.00-143.04   82
  9  \w    -19.00  54.00   0.50   30.00    --   -5.49  35.00 -47.98  146
 10  \w    -20.00   6.00   0.50   30.00    --   -5.49  33.00  45.33   52
 11  \w    -20.00  36.00   0.50   30.00    --   -5.49  33.00 142.30  112
 12  \w    -18.00  27.00   0.50   30.00    --   -5.49 -99.00  90.00   90
 13  \w    -18.00  29.00   0.50   30.00    --   -5.49 -99.00 -60.00   94
 14  \w    -18.00  23.00   0.50   30.00    --   -5.49 -99.00 -90.00   82
 15  \w    -13.00  29.00   0.50   30.00    --   -5.49 -99.00-180.00   84
 16  \w    -64.00  20.00   0.50   30.00    --    4.56 -57.00-180.00  168
 17  \w    -70.00  19.00   0.50   30.00    --    4.56 -33.00  81.66  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0006487000
_diffrn_orient_matrix_UB_12      0.0200686000
_diffrn_orient_matrix_UB_13      0.0459134000
_diffrn_orient_matrix_UB_21      -0.0368473000
_diffrn_orient_matrix_UB_22      -0.0031585000
_diffrn_orient_matrix_UB_23      0.0693936000
_diffrn_orient_matrix_UB_31      0.0202232000
_diffrn_orient_matrix_UB_32      -0.0051203000
_diffrn_orient_matrix_UB_33      0.1374312000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0237
_diffrn_reflns_av_unetI/netI     0.0117
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            36525
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.100
_diffrn_reflns_theta_min         2.171
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.979
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66919
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.12b (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_density_diffrn    2.043
_exptl_crystal_description       plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.681
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 2759 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.027(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         5624
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0187
_refine_ls_R_factor_gt           0.0187
_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^)+(0.0295P)^2^+7.3822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0478
_refine_ls_wR_factor_ref         0.0479
_reflns_Friedel_coverage         0.979
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                5610
_reflns_number_total             5624
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra05697h2.cif
_cod_data_source_block           str0086lt100k
_cod_database_code               7231691
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C10H10N3S2I2
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C9A-C10A \\sim C11A-C12A
 with sigma of 0.005
 C9A-C10A \\sim C11B-C12B
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(C7A) = Uanis(C11A)
Uanis(C7A) = Uanis(C11B)
Uanis(C8A) = Uanis(C12A)
Uanis(C8A) = Uanis(C12B)
Uanis(C9A) = Uanis(C10A)
4. Others
 Sof(H10C)=Sof(H10D)=Sof(C11B)=Sof(H11C)=Sof(H11D)=Sof(C12B)=Sof(H12D)=
 Sof(H12E)=Sof(H12F)=1-FVAR(1)
 Sof(H10A)=Sof(H10B)=Sof(C11A)=Sof(H11A)=Sof(H11B)=Sof(C12A)=Sof(H12A)=
 Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: H4A(0.5) H4B(0.5) H5A(0.5) H5B(0.5) H6A(0.5) H6B(0.5) H7A(0.5)
 H7B(0.5) H8A(0.5) H8B(0.5) H9A(0.5) H9B(0.5) H9C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C7A(H7AA,
 H7AB), C8A(H8AA,H8AB), C9A(H9AA,H9AB), C10A(H10A,H10B), C10A(H10C,H10D),
 C11A(H11A,H11B), C11B(H11C,H11D)
5.b Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C12A(H12A,H12B,H12C), C12B(H12D,H12E,H12F)
;
_shelx_res_checksum              68338
_shelx_fab_checksum              74570
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.438
_oxdiff_exptl_absorpt_empirical_full_min 0.583