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_7043749
_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, C20 H24 Cu N8'
_chemical_formula_sum            'C20 H24 Cl6 Cu N8 Re'
_chemical_formula_weight         838.91
_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   geom
_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                 101.4205(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.69636(15)
_cell_length_b                   14.46868(15)
_cell_length_c                   16.11703(16)
_cell_measurement_reflns_used    20648
_cell_measurement_temperature    120
_cell_measurement_theta_max      30.0930
_cell_measurement_theta_min      3.5900
_cell_volume                     2902.07(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_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      120
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1042
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_details
;
  1 omega  -23.00   19.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3557  -99.0000   90.0000 42

  2 omega  -17.00   17.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3557  -99.0000  150.0000 34

  3 omega  -21.00   12.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3557  -99.0000  -60.0000 33

  4 omega   34.00   80.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745  179.0000 -180.0000 46

  5 omega    2.00   69.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745   57.0000   60.0000 67

  6 omega  -27.00   42.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745  -38.0000 -180.0000 69

  7 omega    4.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745   38.0000  -30.0000 88

  8 omega  -46.00    5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745  -38.0000  150.0000 51

  9 omega  -94.00    4.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3557  -38.0000   60.0000 98

 10 omega  -25.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745  -99.0000   60.0000 90

 11 omega    2.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745   57.0000 -150.0000 90

 12 omega   32.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745 -179.0000  -90.0000 68

 13 omega    2.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745   57.0000  -30.0000 90

 14 omega   34.00   99.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745  179.0000   60.0000 65

 15 omega  -90.00    0.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3557  -57.0000    0.0000 90

 16 omega   -2.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745   38.0000 -120.0000 98

 17 omega  -25.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745  -99.0000  120.0000 90

 18 omega    2.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745   57.0000 -105.0000 90

 19 omega  -46.00   44.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745  -57.0000  -74.0000 90

 20 omega  -25.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745  -99.0000  -90.0000 90

 21 omega  -25.00   21.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3557  -99.0000  -30.0000 46

 22 omega  -86.00   -5.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -21.3557  137.0000  -95.7439 81

 23 omega  -25.00   65.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745  -99.0000 -180.0000 90

 24 omega  -25.00   22.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745  -99.0000  -30.0000 47

 25 omega   -2.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       23.0745   38.0000   60.0000 98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0182991000
_diffrn_orient_matrix_UB_12      -0.0277928000
_diffrn_orient_matrix_UB_13      -0.0305315000
_diffrn_orient_matrix_UB_21      -0.0448294000
_diffrn_orient_matrix_UB_22      -0.0296973000
_diffrn_orient_matrix_UB_23      -0.0017192000
_diffrn_orient_matrix_UB_31      -0.0300760000
_diffrn_orient_matrix_UB_32      0.0273526000
_diffrn_orient_matrix_UB_33      -0.0328797000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            60620
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.814
_diffrn_reflns_theta_min         2.816
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.479
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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            'clear violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.920
_exptl_crystal_description       block
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.1126
_exptl_crystal_size_mid          0.1003
_exptl_crystal_size_min          0.0756
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4403
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0118P)^2^+4.3748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0421
_refine_ls_wR_factor_ref         0.0441
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3787
_reflns_number_total             4403
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02216f2.cif
_cod_data_source_block           eb4199_refinalized
_cod_database_code               7043749
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C30 H30 Re Cl6 N4 Cu'
_chemical_oxdiff_usercomment     '@ 170 K AHP119'
_reflns_odcompleteness_completeness 99.84
_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
2. Rigid body (RIGU) restrains
 C6, C7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7A)=Sof(H7B)=1-FVAR(1)
 Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5A)=Sof(H5B)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11)
4.b X=CH2 refined with riding coordinates:
 C5(H5A,H5B), C7(H7A,H7B), C12(H12A,H12B)
;
_shelx_res_checksum              82392
_olex2_submission_special_instructions 'No special instructions were received'