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_7043752
_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, C28 H48 Cu N8'
_chemical_formula_sum            'C28 H48 Cl6 Cu N8 Re'
_chemical_formula_weight         959.18
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.3832(2)
_cell_length_b                   18.6574(2)
_cell_length_c                   10.60318(13)
_cell_measurement_reflns_used    23596
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.5090
_cell_measurement_theta_min      3.8420
_cell_volume                     3834.54(7)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0521
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
  1 omega  -96.00  -69.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.9518 -179.0000  150.0000 54

  2 omega  -89.00  -62.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.9518 -179.0000  120.0000 54

  3 omega  -27.00    0.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.9518   57.0000   60.0000 54

  4 omega  -30.00   46.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.9518   38.0000 -120.0000 152

  5 omega   44.00   76.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6706   19.0000  -60.0000 64

  6 omega    0.00   95.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6706   77.0000  -60.0000 190

  7 omega    7.00   33.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6706   19.0000  -60.0000 52

  8 omega   20.00   89.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6706   57.0000   30.0000 138

  9 omega   42.00   69.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6706  -99.0000   30.0000 54

 10 omega   23.00   96.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6706   77.0000   90.0000 146

 11 omega  -25.00   69.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6706  -99.0000 -180.0000 188

 12 omega -102.00  -34.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.9518 -179.0000 -180.0000 136

 13 omega  -96.00    4.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.9518  -77.0000   30.0000 200

 14 omega   34.00  104.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6706  179.0000 -150.0000 140

 15 omega    6.00   96.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6706   57.0000 -150.0000 180

 16 omega    6.00   31.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6706   57.0000  -60.0000 50

 17 omega  -41.00   49.00   0.5000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       27.6706  -57.0000  -30.0000 180
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0299682000
_diffrn_orient_matrix_UB_12      -0.0209797000
_diffrn_orient_matrix_UB_13      0.0104979000
_diffrn_orient_matrix_UB_21      0.0208984000
_diffrn_orient_matrix_UB_22      0.0308164000
_diffrn_orient_matrix_UB_23      -0.0087800000
_diffrn_orient_matrix_UB_31      -0.0020043000
_diffrn_orient_matrix_UB_32      0.0074692000
_diffrn_orient_matrix_UB_33      0.0654791000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0174
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            94317
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.636
_diffrn_reflns_theta_min         3.050
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.158
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46067
_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            'pale purple'
_exptl_crystal_density_diffrn    1.661
_exptl_crystal_description       block
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.8702
_exptl_crystal_size_mid          0.2164
_exptl_crystal_size_min          0.1434
_refine_diff_density_max         1.173
_refine_diff_density_min         -0.788
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.329
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         6774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.329
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0203P)^2^+7.2690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0898
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5771
_reflns_number_total             6774
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02216f2.cif
_cod_data_source_block           eb4147_ortho_refinalized
_cod_original_cell_volume        3834.54(8)
_cod_database_code               7043752
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C28 H48 N8 Cl6 Cu Re'
_chemical_oxdiff_usercomment     '@ 170 K AHP029B'
_reflns_odcompleteness_completeness 99.68
_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 C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=1-FVAR(1)
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C11(H11A,H11B), C13(H13A,H13B),
 C15(H15A,H15B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C8(H8), C9(H9), C10(H10)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C)
;
_shelx_res_checksum              33057
_olex2_submission_special_instructions 'No special instructions were received'