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_7043750
_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, 2(C6 H8 Cu0.5 N4), 2(C3 H8 O)'
_chemical_formula_sum            'C18 H32 Cl6 Cu N8 O2 Re'
_chemical_formula_weight         854.95
_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   mixed
_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                76.032(2)
_cell_angle_beta                 80.918(2)
_cell_angle_gamma                69.748(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1219(2)
_cell_length_b                   11.0652(3)
_cell_length_c                   14.7016(4)
_cell_measurement_reflns_used    27189
_cell_measurement_temperature    292.61(10)
_cell_measurement_theta_max      31.0300
_cell_measurement_theta_min      3.4000
_cell_volume                     1494.12(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      air
_diffrn_ambient_temperature      292.61(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1574
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_details
;
  1 omega  -86.00    9.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -38.0000   60.0000 95

  2 omega  -40.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412   57.0000  120.0000 97

  3 omega  -83.00   13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -57.0000  -30.0000 96

  4 omega  -20.00   27.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -99.0000   60.0000 47

  5 omega  -40.00   57.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412   57.0000   30.0000 97

  6 omega  -17.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350   77.0000 -120.0000 105

  7 omega  -84.00  -38.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  151.0000  149.0000 46

  8 omega  -20.00   54.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350  -99.0000 -150.0000 74

  9 omega  -20.00   54.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350  -99.0000  -30.0000 74

 10 omega   15.00   86.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350 -151.0000  106.0000 71

 11 omega   34.00  100.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350 -178.0000    0.0000 66

 12 omega  -86.00  -61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -38.0000  150.0000 25

 13 omega  -20.00   54.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350  -99.0000  150.0000 74

 14 omega   -8.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350   38.0000  150.0000 95
;
_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      0.0087240000
_diffrn_orient_matrix_UB_12      -0.0621660000
_diffrn_orient_matrix_UB_13      0.0304451000
_diffrn_orient_matrix_UB_21      0.0048046000
_diffrn_orient_matrix_UB_22      -0.0286356000
_diffrn_orient_matrix_UB_23      -0.0391777000
_diffrn_orient_matrix_UB_31      0.0742787000
_diffrn_orient_matrix_UB_32      -0.0134715000
_diffrn_orient_matrix_UB_33      -0.0051491000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.924
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48213
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.924
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.208
_diffrn_reflns_theta_min         2.687
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.327
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.998
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.900
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.1915
_exptl_crystal_size_mid          0.1352
_exptl_crystal_size_min          0.0688
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.858
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         8950
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0213
_refine_ls_R_factor_gt           0.0192
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0084P)^2^+0.8626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0361
_refine_ls_wR_factor_ref         0.0367
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8533
_reflns_number_total             8950
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02216f2.cif
_cod_data_source_block           eb4130_refinalized
_cod_original_cell_volume        1494.13(7)
_cod_database_code               7043750
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C12 H16 N8 Cl6 Cu Re'
_chemical_oxdiff_usercomment     '@ 120 K AHP003'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O2-H2
 0.84 with sigma of 0.02
3. Others
 Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17)=Sof(H17)=Sof(H19D)=Sof(H19E)=Sof(H19F)=
 1-FVAR(1)
 Sof(H16A)=Sof(H16B)=Sof(H16C)=Sof(C18)=Sof(H18)=Sof(H19A)=Sof(H19B)=Sof(H19C)=
 FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C14(H14), C17(H17), C18(H18)
4.b Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C16(H16D,H16E,H16F), C19(H19A,H19B,H19C), C19(H19D,H19E,
 H19F)
4.c Aromatic/amide H refined with riding coordinates:
 N2(H2A), C1(H1), C2(H2B), C3(H3), C4(H4A), C5(H5), C6(H6), C7(H7), C8(H8A),
 C9(H9), C10(H10), C11(H11), C12(H12)
4.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              40096
_olex2_submission_special_instructions 'No special instructions were received'