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_7035175
_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         'C20 H20 Br4 Mn N4 O5 Re, C14 H12 N2'
_chemical_formula_sum            'C34 H32 Br4 Mn N6 O5 Re'
_chemical_formula_weight         1165.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 96.1198(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.96409(15)
_cell_length_b                   19.3015(3)
_cell_length_c                   18.0987(3)
_cell_measurement_reflns_used    8315
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.0810
_cell_measurement_theta_min      3.3220
_cell_volume                     3808.28(10)
_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 5.2977
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
  1 omega  -71.00  -15.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5010  -38.0000 -150.0000 56

  2 omega  -69.00   30.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.5010   57.0000   60.0000 99

  3 omega -131.00 -106.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -111.0000 -180.0000 25

  4 omega -128.00  -82.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -61.5000 -111.0000   60.0000 46

  5 omega   65.00  157.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0604   15.0000  -30.0000 92

  6 omega   57.00  150.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0604  178.0000  -90.0000 93

  7 omega   29.00   55.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0604  -30.0000  -60.0000 26

  8 omega   37.00   90.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0604  -30.0000   30.0000 53

  9 omega   29.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0604  -30.0000    0.0000 41

 10 omega   26.00  107.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0604  -94.0000 -120.0000 81

 11 omega   32.00   94.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0604  -45.0000 -120.0000 62

 12 omega   42.00   74.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      107.0604  -45.0000   90.0000 32
;
_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      0.1387785000
_diffrn_orient_matrix_UB_12      0.0076022000
_diffrn_orient_matrix_UB_13      0.0228098000
_diffrn_orient_matrix_UB_21      0.0019173000
_diffrn_orient_matrix_UB_22      0.0659599000
_diffrn_orient_matrix_UB_23      -0.0478044000
_diffrn_orient_matrix_UB_31      -0.0265350000
_diffrn_orient_matrix_UB_32      0.0443320000
_diffrn_orient_matrix_UB_33      0.0672342000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0184
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_laue_measured_fraction_full 1.000
_diffrn_reflns_laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15095
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        66.599
_diffrn_reflns_theta_max         66.599
_diffrn_reflns_theta_min         3.358
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    14.141
_exptl_absorpt_correction_T_max  0.686
_exptl_absorpt_correction_T_min  0.328
_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    2.033
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2232
_exptl_crystal_size_max          0.1632
_exptl_crystal_size_mid          0.1209
_exptl_crystal_size_min          0.0282
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.000076(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         6715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0236
_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^)+(0.0251P)^2^+2.0951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6057
_reflns_number_total             6715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01321f2.cif
_cod_data_source_block           pyc_mn
_cod_depositor_comments
'Adding full bibliography for 7035172--7035176.cif.'
_cod_database_code               7035175
_chemical_oxdiff_formula         'C34 H32 N6 Mn1 Re1 O5 Br4'
_reflns_odcompleteness_completeness 99.97
_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, All O(H,H) groups
2.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C5(H5), C4(H4), C3(H3), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C22(H22), C23(H23), C25(H25), C26(H26), C28(H28), C29(H29)
2.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C33(H33A,H33B,H33C), C34(H34A,H34B,
 H34C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'