Self-assembly of the tetrachlorido(oxalato)rhenate(iv) anion with protonated organic cations: X-ray structures and magnetic properties
Pedersen, Anders H.; Julve, Miguel; Brechin, Euan K.; Martínez-Lillo, José; CrystEngComm 19 (2017) 503–; doi:10.1039/C6CE02025A

data_7227258
_publ_section_title
;
 Self-assembly of the tetrachlorido(oxalato)rhenate(iv) anion with
 protonated organic cations: X-ray structures and magnetic properties
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              503
_journal_paper_doi               10.1039/C6CE02025A
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C2 Cl4 O4 Re, C10 H10 N2'
_chemical_formula_sum            'C12 H10 Cl4 N2 O4 Re'
_chemical_formula_weight         574.22
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-09-09 deposited with the CCDC.
2016-12-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 113.592(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.3070(3)
_cell_length_b                   17.6267(4)
_cell_length_c                   10.8072(3)
_cell_measurement_reflns_used    9109
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      75.9900
_cell_measurement_theta_min      5.0270
_cell_volume                     1624.75(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -50.00   29.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000 -120.0000 79

  2 omega -116.00  -21.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -38.0000 -120.0000 95

  3 omega  -50.00   29.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000   30.0000 79

  4 omega -114.00  -62.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686 -143.0000  -23.0000 52

  5 omega  -96.00   -2.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  125.0000  120.0000 94

  6 omega    1.00   83.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       43.1686  -99.0000   30.0000 82

  7 omega   30.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -90.0000 79

  8 omega   40.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000  -60.0000 59

  9 omega   39.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000 -180.0000 82

 10 omega   87.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000   90.0000 91

 11 omega   87.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000   30.0000 91

 12 omega   39.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000   30.0000 82

 13 omega   30.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -150.0000 79

 14 omega   87.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   30.0000  -60.0000 91

 15 omega   36.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000  150.0000 55

 16 omega   30.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000   30.0000 79

 17 omega   39.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -30.0000 82

 18 omega   40.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -45.0000    0.0000 59

 19 omega   80.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   77.0000  120.0000 98

 20 omega   39.00  121.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000 -125.0000  -60.0000 82

 21 omega   93.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  127.0000 -138.0000 85

 22 omega   30.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  -30.0000 79

 23 omega   30.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000  150.0000 79

 24 omega   36.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -30.0000   30.0000 55

 25 omega   30.00  109.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  -94.0000 -180.0000 79

 26 omega   87.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000   45.0000    0.0000 91

 27 omega   94.00  178.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      111.0000  125.0000  -60.0000 84

 28 omega -117.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000    0.0000 105

 29 omega -113.00  -17.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000 -180.0000 96

 30 omega  -50.00   29.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686   38.0000  -30.0000 79

 31 omega -117.00  -12.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -77.0000   90.0000 105

 32 omega -113.00  -17.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -43.1686  -57.0000   90.0000 96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0150839000
_diffrn_orient_matrix_UB_12      0.0870688000
_diffrn_orient_matrix_UB_13      0.0083593000
_diffrn_orient_matrix_UB_21      -0.0919403000
_diffrn_orient_matrix_UB_22      0.0054168000
_diffrn_orient_matrix_UB_23      -0.1540335000
_diffrn_orient_matrix_UB_31      -0.1547988000
_diffrn_orient_matrix_UB_32      0.0052977000
_diffrn_orient_matrix_UB_33      0.0196650000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12929
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.306
_diffrn_reflns_theta_min         5.018
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.879
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.347
_exptl_crystal_description       plate
_exptl_crystal_F_000             1084
_exptl_crystal_preparation       ', Magnetic properties'
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.4829
_exptl_crystal_size_mid          0.0565
_exptl_crystal_size_min          0.0197
_refine_diff_density_max         2.788
_refine_diff_density_min         -1.231
_refine_diff_density_rms         0.198
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0686P)^2^+3.6307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1661
_reflns_number_total             1700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ce02025a2.cif
_cod_data_source_block           eb15144_refinalized
_cod_depositor_comments
'Adding full bibliography for 7227258--7227259.cif.'
_cod_database_code               7227258
_chemical_oxdiff_formula         'C12 H8 Cl4 N2 O4'
_chemical_oxdiff_usercomment     '@ 120 K AHP261C'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2A), C3(H3), C6(H6), C7(H7)
;
_shelx_res_checksum              34509
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'