Magneto-structural correlations in a family of ReIVCuII chains based on the hexachlororhenate(IV) metalloligand
Brechin, Euan K.; Pedersen, Anders Hjordt H.; Julve, Miguel; Martínez-Lillo, José; Cano, Joan; Dalton Trans.  (2017) –; doi:10.1039/C7DT02216F

data_7043753
_publ_section_title
;
 Magneto-structural correlations in a family of ReIVCuII chains based on
 the hexachlororhenate(IV) metalloligand
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02216F
_journal_year                    2017
_chemical_formula_moiety         'Cl6 Re, C12 H28 Cu N4 O4, C2 H3 N'
_chemical_formula_sum            'C14 H31 Cl6 Cu N5 O4 Re'
_chemical_formula_weight         795.88
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-05-16 deposited with the CCDC.
2017-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                95.043(2)
_cell_angle_beta                 91.8824(19)
_cell_angle_gamma                90.111(2)
_cell_formula_units_Z            1
_cell_length_a                   8.46428(19)
_cell_length_b                   8.5772(2)
_cell_length_c                   9.7582(2)
_cell_measurement_reflns_used    13990
_cell_measurement_temperature    119.99(10)
_cell_measurement_theta_max      30.9830
_cell_measurement_theta_min      3.9050
_cell_volume                     705.31(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      119.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_details
;
  1 omega  -20.00   27.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.3975  -99.0000    0.0000 47

  2 omega  -79.00  -33.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.3975  142.0000   91.5148 46

  3 omega   34.00  100.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912 -178.0000 -150.0000 66

  4 omega  -20.00   54.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912  -99.0000  -90.0000 74

  5 omega  -58.00   37.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912  -38.0000 -120.0000 95

  6 omega   -8.00   87.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912   38.0000   30.0000 95

  7 omega  -58.00   37.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4912  -38.0000 -150.0000 95

  8 omega  -84.00   13.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.3975  -57.0000 -150.0000 97

  9 omega  -20.00   27.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.3975  -99.0000   90.0000 47

 10 omega  -86.00    9.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.3975  -38.0000   60.0000 95

 11 omega  -73.00  -27.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.3975  132.0000  -72.7082 46

 12 omega  -45.00   60.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.3975   77.0000    0.0000 105
;
_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      0.0072255000
_diffrn_orient_matrix_UB_12      -0.0679183000
_diffrn_orient_matrix_UB_13      0.0362418000
_diffrn_orient_matrix_UB_21      -0.0830623000
_diffrn_orient_matrix_UB_22      -0.0112632000
_diffrn_orient_matrix_UB_23      -0.0060207000
_diffrn_orient_matrix_UB_31      0.0088605000
_diffrn_orient_matrix_UB_32      -0.0463934000
_diffrn_orient_matrix_UB_33      -0.0630936000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.911
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            19023
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.911
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.216
_diffrn_reflns_theta_min         3.140
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.637
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.2629
_exptl_crystal_size_mid          0.1633
_exptl_crystal_size_min          0.1397
_refine_diff_density_max         2.805
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         4179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0204
_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^)+(0.0234P)^2^+0.5259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0473
_refine_ls_wR_factor_ref         0.0475
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4133
_reflns_number_total             4179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02216f2.cif
_cod_data_source_block           eb4261_refinalized
_cod_database_code               7043753
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C12 H28 Cl6 Cu N4 O4'
_chemical_oxdiff_usercomment     '@ 120 K AHP186C'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: N3(0.5) C7(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
 H8B,H8C)
;
_shelx_res_checksum              90144
_olex2_submission_special_instructions 'No special instructions were received'