Magneto-structural correlations in dirhenium(IV) complexes possessing magnetic pathways with even or odd numbers of atoms.
Brechin, Euan K.; Pedersen, Anders Hjordt H.; Julve, Miguel; Martínez-Lillo, José; Cano, Joan; Dalton Trans.  (2017) –; doi:10.1039/C7DT02612A

data_7043981
_publ_section_title
;
 Magneto-structural correlations in dirhenium(IV) complexes possessing
 magnetic pathways with even or odd numbers of atoms.
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02612A
_journal_year                    2017
_chemical_formula_moiety         'C4 H4 Br10 N2 Re2, 2(C16 H36 N)'
_chemical_formula_sum            'C36 H76 Br10 N4 Re2'
_chemical_formula_weight         1736.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-06-21 deposited with the CCDC.
2017-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.122(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5547(3)
_cell_length_b                   15.1382(2)
_cell_length_c                   21.5926(3)
_cell_measurement_reflns_used    22975
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.1180
_cell_measurement_theta_min      3.6330
_cell_volume                     5411.27(14)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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    'SIR2004 (Burla et al., 2007)'
_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 0.998
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -25.00  25.00   0.50   13.00    --  -17.08 -99.00   0.00  100
  2  \w    -37.00  52.00   0.50   13.00    --  -17.08  57.00   0.00  178
  3  \w    -86.00   4.00   0.50   13.00    --  -17.08 -57.00-120.00  180
  4  \w    -93.00 -34.00   0.50   13.00    --  -17.08-179.00 -60.00  118
  5  \w    -25.00  62.00   0.50   13.00    --   19.73 -99.00 150.00  174
  6  \w    -10.00  90.00   0.50   13.00    --   19.73  77.00-150.00  200
  7  \w     -6.00  92.00   0.50   13.00    --   19.73  37.00   0.00  196
  8  \w    -25.00  25.00   0.50   13.00    --  -17.08 -99.00  60.00  100
  9  \w    -90.00  26.00   0.50   13.00    --  -17.08   0.00 -30.00  232
 10  \w    -53.00  46.00   0.50   13.00    --   19.73 -37.00-150.00  198
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0347173000
_diffrn_orient_matrix_UB_12      -0.0043410000
_diffrn_orient_matrix_UB_13      -0.0189486000
_diffrn_orient_matrix_UB_21      -0.0249754000
_diffrn_orient_matrix_UB_22      -0.0103102000
_diffrn_orient_matrix_UB_23      -0.0257271000
_diffrn_orient_matrix_UB_31      -0.0023560000
_diffrn_orient_matrix_UB_32      0.0455133000
_diffrn_orient_matrix_UB_33      -0.0076305000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0941
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            94121
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.161
_diffrn_reflns_theta_min         2.958
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    11.882
_exptl_absorpt_correction_T_max  0.9383
_exptl_absorpt_correction_T_min  0.3180
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1057 before and 0.0560 after correction.
The Ratio of minimum to maximum transmission is 0.3389.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.132
_exptl_crystal_description       plate
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.695
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.044
_refine_diff_density_max         1.411
_refine_diff_density_min         -1.219
_refine_diff_density_rms         0.186
_refine_ls_abs_structure_details
;
 Flack x determined using 6895 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.031(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         25646
_refine_ls_number_restraints     421
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0280P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0769
_reflns_Friedel_coverage         0.840
_reflns_Friedel_fraction_full    0.990
_reflns_Friedel_fraction_max     0.832
_reflns_number_gt                18840
_reflns_number_total             25646
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02612a2.cif
_cod_data_source_block           eb4159
_cod_database_code               7043981
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C4 H4 Br6 N2 Re'
_chemical_oxdiff_usercomment     '@ 170 K AHP153'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 N7, C52, C55, C57, C48, C56, C43, C51, C44, C47, C49, C45, C53, C46, C50, C54,
  C58
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N6, C39, C35, C41, C40, C36, C31, C32, C27, C38, C37, C42, C28, C33, C34, C30,
  C29
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N8, C69, C71, C64, C59, C67, C60, C68, C61, C63, C73, C65, C72, C74, C62, C66,
  C70
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N5, C10, H10A, H10B, C17, H17A, H17B, C11, H11A, H11B, C13, H13A, H13B, C9,
 H9A, H9B, C21, H21A, H21B, C16, H16A, H16B, H16C, C14, H14A, H14B, C12, H12A,
 H12B, H12C, C22, C18, H18A, H18B, C19, H19A, H19B, C15, H15A, H15B, C20, H20A,
 H20B, H20C, C24, C23, C26, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(H22C)=Sof(H22D)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=1-FVAR(1)
 Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B),
 C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C21(H21A,H21B),
  C22(H22A,H22B), C22(H22C,H22D), C23(H23A,H23B), C25(H25A,H25B), C27(H27A,
 H27B), C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B), C32(H32A,H32B),
 C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C39(H39A,H39B),
  C40(H40A,H40B), C41(H41A,H41B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,
 H45B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C51(H51A,H51B),
 C52(H52A,H52B), C53(H53A,H53B), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B),
  C59(H59A,H59B), C60(H60A,H60B), C61(H61A,H61B), C63(H63A,H63B), C64(H64A,
 H64B), C65(H65A,H65B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B),
 C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C34(H34A,H34B,H34C), C38(H38A,
 H38B,H38C), C42(H42A,H42B,H42C), C46(H46A,H46B,H46C), C50(H50A,H50B,H50C),
 C54(H54A,H54B,H54C), C58(H58A,H58B,H58C), C62(H62A,H62B,H62C), C66(H66A,H66B,
 H66C), C70(H70A,H70B,H70C), C74(H74A,H74B,H74C)
;
_shelx_res_checksum              7008
_olex2_submission_special_instructions 'No special instructions were received'