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_7035172
_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         'C6 H5 Br4 N2 O3 Re, C16 H36 N'
_chemical_formula_sum            'C22 H41 Br4 N3 O3 Re'
_chemical_formula_weight         901.42
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-03-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-03-24 deposited with the CCDC.
2015-05-14 downloaded from the CCDC.
;
_cell_angle_alpha                83.720(3)
_cell_angle_beta                 74.333(3)
_cell_angle_gamma                69.949(3)
_cell_formula_units_Z            4
_cell_length_a                   11.8626(4)
_cell_length_b                   14.7096(5)
_cell_length_c                   20.6473(7)
_cell_measurement_reflns_used    9505
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      66.5945
_cell_measurement_theta_min      3.1988
_cell_volume                     3258.2(2)
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
  1 omega  -54.00   41.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.3475   67.0000  -75.0000 95

  2 omega    3.00  117.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       38.3475   67.0000   28.0000 114

  3 omega  -14.00   66.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       38.3475  -67.0000  151.0000 80

  4 omega   11.00   36.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       38.3475   67.0000  104.0000 25

  5 omega -115.00  -90.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000  -67.0000  -28.0000 25

  6 omega  110.00  162.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389   67.0000   28.0000 52

  7 omega   30.00  144.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389  -67.0000  151.0000 114

  8 omega   57.00   91.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389  -67.0000   75.0000 34

  9 omega   74.00  101.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389   67.0000  104.0000 27

 10 omega  -42.00  -10.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.3475  -38.0000   60.0000 32

 11 omega -114.00  -28.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.3475  -57.0000 -180.0000 86

 12 omega   36.00   97.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       38.3475 -125.0000   90.0000 61

 13 omega  -75.00  -43.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -68.5000  -45.0000   90.0000 32

 14 omega   29.00   83.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389  -30.0000  150.0000 54

 15 omega   74.00  111.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389   77.0000  120.0000 37

 16 omega   80.00  168.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389   45.0000  -30.0000 88

 17 omega   29.00   58.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389  -30.0000   90.0000 29

 18 omega   43.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389  -45.0000  -30.0000 52

 19 omega  126.00  177.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389   77.0000  120.0000 51

 20 omega   72.00   98.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389  178.0000    0.0000 26

 21 omega  111.00  149.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389  178.0000    0.0000 38

 22 omega   81.00  176.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389   45.0000   90.0000 95

 23 omega   35.00  108.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389  -94.0000  -30.0000 73

 24 omega  153.00  178.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389  111.0000 -180.0000 25

 25 omega   86.00  172.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      108.8389   30.0000 -180.0000 86
;
_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      0.0842575000
_diffrn_orient_matrix_UB_12      -0.0174528000
_diffrn_orient_matrix_UB_13      0.0484457000
_diffrn_orient_matrix_UB_21      0.0850048000
_diffrn_orient_matrix_UB_22      -0.0949963000
_diffrn_orient_matrix_UB_23      -0.0358136000
_diffrn_orient_matrix_UB_31      0.0777864000
_diffrn_orient_matrix_UB_32      0.0557258000
_diffrn_orient_matrix_UB_33      -0.0487603000
_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     0.0312
_diffrn_reflns_laue_measured_fraction_full 0.977
_diffrn_reflns_laue_measured_fraction_max 0.977
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            22869
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_theta_full        66.595
_diffrn_reflns_theta_max         66.595
_diffrn_reflns_theta_min         3.199
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.239
_exptl_absorpt_correction_T_max  0.662
_exptl_absorpt_correction_T_min  0.417
_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    1.838
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1732
_exptl_crystal_size_max          0.0983
_exptl_crystal_size_mid          0.0756
_exptl_crystal_size_min          0.0344
_refine_diff_density_max         0.684
_refine_diff_density_min         -0.732
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     625
_refine_ls_number_reflns         11247
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0316
_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^)+(0.0275P)^2^+2.2741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9083
_reflns_number_total             11247
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01321f2.cif
_cod_data_source_block           pyc_re
_cod_depositor_comments
'Adding full bibliography for 7035172--7035176.cif.'
_cod_original_cell_volume        3258.1(2)
_cod_database_code               7035172
_chemical_oxdiff_formula         'C44 H79 Br8 N6 O6 Re2'
_reflns_odcompleteness_completeness 97.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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, All O(H) groups
2. Others
 Sof(H33C)=Sof(H33D)=Sof(C34D)=Sof(H34A)=Sof(H34B)=Sof(H34C)=1-FVAR(1)
 Sof(H33A)=Sof(H33B)=Sof(C35D)=Sof(H35A)=Sof(H35B)=Sof(H35C)=FVAR(1)
 Sof(H43A)=Sof(H43B)=Sof(C44D)=Sof(H44A)=Sof(H44B)=Sof(H44C)=1-FVAR(2)
 Sof(H43C)=Sof(H43D)=Sof(C45D)=Sof(H45A)=Sof(H45B)=Sof(H45C)=FVAR(2)
3.a Secondary CH2 refined with riding coordinates:
 C11C(H11C,H11D), C12C(H12C,H12D), C13C(H13C,H13D), C21C(H21C,H21D), C22C(H22C,
 H22D), C23C(H23C,H23D), C31C(H31C,H31D), C32C(H32C,H32D), C33C(H33E,H33F),
 C41C(H41C,H41D), C42C(H42C,H42D), C43C(H43E,H43F), C11D(H11A,H11B), C12D(H12A,
 H12B), C13D(H13A,H13B), C21D(H21A,H21B), C22D(H22A,H22B), C23D(H23A,H23B),
 C31D(H31A,H31B), C32D(H32A,H32B), C33D(H33A,H33B), C33D(H33C,H33D), C41D(H41A,
 H41B), C42D(H42A,H42B), C43D(H43C,H43D), C43D(H43A,H43B)
3.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C3A(H3AA), C4A(H4A), C5A(H5A), C1B(H1B), C3B(H3B), C4B(H4B), C5B(H5B)
3.c Tetrahedral OH refined with riding coordinates:
 O3A(H3A), O2B(H2B)
3.d Idealised Me refined as rotating group:
 C14C(H14D,H14E,H14F), C24C(H24D,H24E,H24F), C34C(H34D,H34E,H34F), C44C(H44D,
 H44E,H44F), C14D(H14A,H14B,H14C), C24D(H24A,H24B,H24C), C35D(H35A,H35B,H35C),
 C45D(H45A,H45B,H45C), C34D(H34A,H34B,H34C), C44D(H44A,H44B,H44C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'