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_7043980
_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         'C3 H3 Br10 N3 Re2, 2(C16 H36 N)'
_chemical_formula_sum            'C35 H75 Br10 N5 Re2'
_chemical_formula_weight         1737.50
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
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Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
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2017-06-21 deposited with the CCDC.
2017-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
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_cell_length_c                   20.8616(5)
_cell_measurement_reflns_used    21979
_cell_measurement_temperature    120.00(10)
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_cell_measurement_theta_min      3.3700
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
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_diffrn_ambient_environment      N~2~
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_diffrn_measurement_details
;
  1 omega  -36.00   59.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412   38.0000  -30.0000 190

  2 omega  -86.00    9.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -38.0000   90.0000 190

  3 omega  -20.00   27.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -99.0000 -180.0000 94

  4 omega  -20.00   27.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -99.0000   60.0000 94

  5 omega  -83.00   13.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -57.0000 -180.0000 192

  6 omega  -92.00   24.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -19.0000  -30.0000 232

  7 omega  -20.00   27.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -99.0000   90.0000 94

  8 omega  -86.00    9.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -38.0000 -180.0000 190

  9 omega  -56.00   41.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350  -57.0000  -60.0000 194

 10 omega   34.00  100.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350 -178.0000  120.0000 132

 11 omega  -86.00  -61.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.2412  -38.0000  -90.0000 50

 12 omega   34.00  100.00   0.5000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       14.3350 -178.0000 -120.0000 132
;
_diffrn_measurement_device       'four-circle diffractometer'
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_diffrn_orient_matrix_UB_13      -0.0198950000
_diffrn_orient_matrix_UB_21      0.0074836000
_diffrn_orient_matrix_UB_22      0.0138081000
_diffrn_orient_matrix_UB_23      -0.0295050000
_diffrn_orient_matrix_UB_31      0.0053868000
_diffrn_orient_matrix_UB_32      -0.0617880000
_diffrn_orient_matrix_UB_33      -0.0041486000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            66891
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.949
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.081
_diffrn_reflns_theta_min         2.977
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    12.308
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35e (release 07-10-2014 CrysAlis171 .NET)
(compiled Oct  7 2014,17:20:27)
Numerical absorption correction based on gaussian integration over
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Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.209
_exptl_crystal_description       block
_exptl_crystal_F_000             3280
_exptl_crystal_size_max          0.2064
_exptl_crystal_size_mid          0.1075
_exptl_crystal_size_min          0.0769
_refine_diff_density_max         1.102
_refine_diff_density_min         -1.557
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
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_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0275
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_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0113P)^2^+8.1642P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0436
_refine_ls_wR_factor_ref         0.0453
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7101
_reflns_number_total             7965
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02612a2.cif
_cod_data_source_block           eb15001_refinalized
_cod_original_cell_volume        5224.26(19)
_cod_database_code               7043980
_chemical_oxdiff_formula         'C3 H3 Br6 N3 Re'
_chemical_oxdiff_usercomment     '@ 120 K AHP211-DCM'
_reflns_odcompleteness_completeness 99.82
_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.a Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C4(H4a,H4b), C5(H5a,H5b), C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b),
 C11(H11a,H11b), C12(H12a,H12b), C13(H13a,H13b), C15(H15a,H15b), C16(H16a,H16b),
  C17(H17a,H17b)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
2.c Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C10(H10a,H10b,H10c), C14(H14a,H14b,H14c), C18(H18a,H18b,H18c)
;
_shelx_res_checksum              83935
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'