The crystal structure and magnetic properties of 3-pyridinecarboxylate-bridged Re(ii)M(ii) complexes (M = Cu, Ni, Co and Mn).
Pacheco, Mario; Cuevas, Alicia; González-Platas, Javier; Lloret, Francesc; Julve, Miguel; Kremer, Carlos; Dalton transactions (Cambridge, England : 2003) 44 (2015) 11636–11648; doi:10.1039/c5dt01321f

data_7035173
_publ_section_title
;
 The crystal structure and magnetic properties of
 3-pyridinecarboxylate-bridged Re(ii)M(ii) complexes (M = Cu, Ni, Co and
 Mn).
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11636
_journal_page_last               11648
_journal_paper_doi               10.1039/c5dt01321f
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         '2(C34 H28 Br4 N6 Ni O3 Re), C2 H3 N'
_chemical_formula_sum            'C70 H59 Br8 N13 Ni2 O6 Re2'
_chemical_formula_weight         2307.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-23 deposited with the CCDC.
2015-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.2729(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.74860(10)
_cell_length_b                   19.72731(14)
_cell_length_c                   18.11565(14)
_cell_measurement_reflns_used    18754
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.5880
_cell_measurement_theta_min      3.4089
_cell_volume                     3986.91(6)
_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, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5953
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -29.00   -2.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.6776  125.0000 -150.0000 27

  2 omega  -46.00   35.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.6776   38.0000 -180.0000 81

  3 omega -129.00   48.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -40.6776    0.0000  120.0000 177

  4 omega   68.00  101.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.6776   38.0000  -60.0000 33

  5 omega   38.00   77.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.6776 -125.0000 -180.0000 39

  6 omega   30.00   93.00   1.0000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       40.6776 -125.0000   90.0000 63

  7 omega   38.00  106.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338 -125.0000 -150.0000 68

  8 omega   37.00   79.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338  -30.0000   60.0000 42

  9 omega   51.00   97.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338  -61.0000   60.0000 46

 10 omega   81.00  146.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338   45.0000  -90.0000 65

 11 omega   98.00  142.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338  125.0000  120.0000 44

 12 omega  146.00  175.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338  125.0000  120.0000 29

 13 omega   78.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338   30.0000  -30.0000 99

 14 omega   87.00  121.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338 -125.0000  120.0000 34

 15 omega   38.00   77.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338 -125.0000  120.0000 39

 16 omega   80.00  176.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338   77.0000 -180.0000 96

 17 omega   96.00  131.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338   81.0000  114.0000 35

 18 omega   80.00  172.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338   45.0000 -120.0000 92

 19 omega   51.00   86.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338   15.0000 -120.0000 35

 20 omega  108.00  167.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338  125.0000   90.0000 59

 21 omega   30.00  101.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      107.6338  -94.0000   30.0000 71
;
_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      -0.1106516000
_diffrn_orient_matrix_UB_12      0.0403841000
_diffrn_orient_matrix_UB_13      0.0030962000
_diffrn_orient_matrix_UB_21      -0.0248270000
_diffrn_orient_matrix_UB_22      -0.0537086000
_diffrn_orient_matrix_UB_23      0.0547606000
_diffrn_orient_matrix_UB_31      0.0787769000
_diffrn_orient_matrix_UB_32      0.0397953000
_diffrn_orient_matrix_UB_33      0.0707907000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0164
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27246
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.588
_diffrn_reflns_theta_max         66.588
_diffrn_reflns_theta_min         3.409
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.474
_exptl_absorpt_correction_T_max  0.558
_exptl_absorpt_correction_T_min  0.114
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2208
_exptl_crystal_size_max          0.3174
_exptl_crystal_size_mid          0.2854
_exptl_crystal_size_min          0.0591
_refine_diff_density_max         1.333
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7024
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0322
_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^)+(0.0346P)^2^+9.1960P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0842
_refine_ls_wR_factor_ref         0.0851
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6768
_reflns_number_total             7024
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01321f2.cif
_cod_data_source_block           pyc_ni
_cod_depositor_comments
'Adding full bibliography for 7035172--7035176.cif.'
_cod_database_code               7035173
_chemical_oxdiff_formula         'C70 H59 Br8 N13 Ni2 O6 Re2'
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C35-C36
 1.5 with sigma of 0.02
 C36-N7
 1.2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C35 \\sim C36 \\sim N7: within 1.5A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Others
 Fixed Sof: N7(0.5) C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5) C36(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29)
5.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'