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_7231692
_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         'C18 H13 N7 S2'
_chemical_formula_sum            'C18 H13 N7 S2'
_chemical_formula_weight         391.47
_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
_audit_creation_date             2018-09-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-09-18 deposited with the CCDC.
2018-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                79.7400(10)
_cell_angle_beta                 66.715(2)
_cell_angle_gamma                73.107(2)
_cell_formula_units_Z            8
_cell_length_a                   15.8211(3)
_cell_length_b                   15.8245(3)
_cell_length_c                   16.6689(2)
_cell_measurement_reflns_used    21426
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0860
_cell_measurement_theta_min      2.8850
_cell_volume                     3658.41(12)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.988
_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    -43.00  23.00   0.50    2.00    --  -46.12  34.00 105.00  132
  2  \w    -45.00 -19.00   0.50    3.99    --  -88.50 125.00 150.00   52
  3  \w    -74.00 -12.00   0.50    3.99    --  -88.50  34.00 105.00  124
  4  \w    -85.00 -58.00   0.50    3.99    --  -88.50 125.00 150.00   54
  5  \w    -85.00 -60.00   0.50    3.99    --  -88.50  45.00 -60.00   50
  6  \w   -121.00 -55.00   0.50    2.00    --  -46.12 -34.00 -52.00  132
  7  \w    -28.00  44.00   0.50    2.00    --   46.12 -34.00 -52.00  144
  8  \w     30.00  59.00   0.50    3.99    --  105.44 -34.00 -52.00   58
  9  \w     31.00  59.00   0.50    3.99    --  105.44 -30.00   0.00   56
 10  \w     39.00  65.00   0.50    3.99    --  105.44 -45.00  60.00   52
 11  \w     37.00  65.00   0.50    3.99    --  105.44 -45.00 120.00   56
 12  \w     36.00  61.00   0.50    3.99    --  105.44 -45.00 150.00   50
 13  \w     31.00  58.00   0.50    3.99    --  105.44 -30.00 120.00   54
 14  \w     32.00  58.00   0.50    3.99    --  105.44 -30.00 150.00   52
 15  \w     32.00  57.00   0.50    3.99    --  105.44 -45.00  90.00   50
 16  \w     30.00  55.00   0.50    3.99    --  105.44 -30.00  30.00   50
 17  \w     89.00 178.00   0.50    3.99    --  105.44  34.00 105.00  178
 18  \w    109.00 177.00   0.50    3.99    --  105.44  30.00 -30.00  136
 19  \w    149.00 178.00   0.50    3.99    --  105.44 125.00   0.00   58
 20  \w    100.00 126.00   0.50    3.99    --  105.44 125.00-150.00   52
 21  \w    139.00 170.00   0.50    3.99    --  105.44 125.00-150.00   62
 22  \w    101.00 133.00   0.50    3.99    --  105.44 125.00   0.00   64
 23  \w     88.00 172.00   0.50    3.99    --  105.44  61.00   0.00  168
 24  \w     85.00 110.00   0.50    2.00    --   46.12  77.00-150.00   50
 25  \w     30.00  57.00   0.50    3.99    --  105.44 -30.00-150.00   54
 26  \w     33.00  59.00   0.50    3.99    --  105.44 -30.00 -90.00   52
 27  \w     32.00 126.00   0.50    3.99    --  105.44 -77.00 -90.00  188
 28  \w     92.00 118.00   0.50    3.99    --  105.44-125.00 -30.00   52
 29  \w     71.00 107.00   0.50    3.99    --  105.44-125.00  30.00   72
 30  \w     74.00 118.00   0.50    3.99    --  105.44-125.00  60.00   88
 31  \w     38.00  65.00   0.50    2.00    --   46.12 -77.00  90.00   54
 32  \w     30.00  95.00   0.50    2.00    --   46.12-125.00 -30.00  130
 33  \w     41.00  85.00   0.50    3.99    --  105.44 -94.00  30.00   88
 34  \w     38.00  63.00   0.50    3.99    --  105.44-125.00  30.00   50
 35  \w     32.00 108.00   0.50    3.99    --  105.44 -94.00  60.00  152
 36  \w     33.00 107.00   0.50    3.99    --  105.44 -94.00 -90.00  148
 37  \w     67.00 115.00   0.50    3.99    --  105.44-125.00-120.00   96
 38  \w     33.00  62.00   0.50    3.99    --  105.44-125.00 -30.00   58
 39  \w     -6.00  24.00   0.50    2.00    --   46.12 -77.00  90.00   60
 40  \w     36.00  82.00   0.50    3.99    --  105.44 -94.00 150.00   92
 41  \w     30.00 120.00   0.50    2.00    --   46.12  34.00 105.00  180
 42  \w     31.00  57.00   0.50    3.99    --  105.44 -30.00-180.00   52
 43  \w     38.00  63.00   0.50    3.99    --  105.44 -45.00-180.00   50
 44  \w     38.00 116.00   0.50    3.99    --  105.44-125.00-180.00  156
 45  \w   -118.00 -92.00   0.50    2.00    --  -46.12-125.00 120.00   52
 46  \w   -156.00 -95.00   0.50    3.99    --  -88.50 -34.00 -52.00  122
 47  \w   -119.00 -94.00   0.50    2.00    --  -46.12 -77.00-150.00   50
 48  \w   -113.00 -87.00   0.50    2.00    --  -46.12 -77.00-180.00   52
 49  \w   -103.00 -78.00   0.50    2.00    --  -46.12-125.00 -60.00   50
;
_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      0.0261447000
_diffrn_orient_matrix_UB_12      -0.0951531000
_diffrn_orient_matrix_UB_13      0.0395691000
_diffrn_orient_matrix_UB_21      -0.1005092000
_diffrn_orient_matrix_UB_22      -0.0097466000
_diffrn_orient_matrix_UB_23      0.0195687000
_diffrn_orient_matrix_UB_31      0.0340756000
_diffrn_orient_matrix_UB_32      -0.0354475000
_diffrn_orient_matrix_UB_33      -0.0907069000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0754
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48939
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.129
_diffrn_reflns_theta_min         2.894
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.794
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61010
_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            'metallic dark black'
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       plate
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.015
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     977
_refine_ls_number_reflns         14247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+1.0624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1139
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12073
_reflns_number_total             14247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra05697h2.cif
_cod_data_source_block           str0040lt100k
_cod_database_code               7231692
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C20H20N8S2
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.767
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C13C(H13G,H13H), C14C(H14G,H14H), C15C(H15G,H15H), C16C(H16G,H16H), C17C(H17G,
 H17H), C13(H13A,H13B), C13A(H13C,H13D), C13B(H13E,H13F), C14(H14A,H14B),
 C14A(H14C,H14D), C14B(H14E,H14F), C15(H15A,H15B), C15A(H15C,H15D), C15B(H15E,
 H15F), C16(H16A,H16B), C16A(H16C,H16D), C16B(H16E,H16F), C17(H17A,H17B),
 C17A(H17C,H17D), C17B(H17E,H17F)
2.b Idealised Me refined as rotating group:
 C18C(H18J,H18K,H18L), C18(H18A,H18B,H18C), C18A(H18D,H18E,H18F), C18B(H18G,
 H18H,H18I)
;
_shelx_res_checksum              94221
_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 1.842
_oxdiff_exptl_absorpt_empirical_full_min 0.395