M(ii) (M = Mn, Co, Ni) variants of the MIL-53-type structure with pyridine-N-oxide as a co-ligand
Munn, Alexis S.; Clarkson, Guy J.; Millange, Franck; Dumont, Yves; Walton, Richard I.; CrystEngComm 15 (2013) 9679–; doi:10.1039/c3ce41268g

data_7211122
_publ_section_title
;
 M(ii) (M = Mn, Co, Ni) variants of the MIL-53-type structure with
 pyridine-N-oxide as a co-ligand
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              9679
_journal_paper_doi               10.1039/c3ce41268g
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C13 H9 Co0.84 Mn0.16 N O5'
_chemical_formula_sum            'C13 H9 Co0.84 Mn0.16 N O5'
_chemical_formula_weight         317.50
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-06-06
_audit_creation_method
;
  Olex2 1.2
  (compiled 2013.04.25 svn.r2679, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.70(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.400(9)
_cell_length_b                   9.284(9)
_cell_length_c                   7.130(7)
_cell_measurement_reflns_used    41
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.1987
_cell_measurement_theta_min      2.9957
_cell_volume                     1279.1(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
  1 omega    2.00   30.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       11.0058  -57.0000 -150.0000 28

  2 omega  -51.00   31.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       11.0058  -38.0000  150.0000 82

  3 omega   16.00   80.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       11.0058   57.0000   60.0000 64

  4 omega  -58.00   38.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       11.0058  -57.0000  -90.0000 96

  5 omega  -20.00   28.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9433  -99.0000  -60.0000 48

  6 omega  -98.00  -72.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9433  178.0000   90.0000 26

  7 omega  -98.00  -69.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9433  178.0000   30.0000 29

  8 omega  -79.00  -53.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9433  178.0000    0.0000 26

  9 omega   35.00   98.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       11.0058  178.0000  120.0000 63

 10 omega  -12.00   84.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       11.0058   38.0000 -180.0000 96

 11 omega  -59.00   38.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       11.0058  -57.0000  120.0000 97

 12 omega  -20.00   85.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       11.0058   77.0000 -120.0000 105

 13 omega  -59.00  -26.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9433  111.0000 -109.0000 33
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0109112000
_diffrn_orient_matrix_UB_12      0.0757085000
_diffrn_orient_matrix_UB_13      0.0047503000
_diffrn_orient_matrix_UB_21      0.0941831000
_diffrn_orient_matrix_UB_22      -0.0051815000
_diffrn_orient_matrix_UB_23      -0.0102884000
_diffrn_orient_matrix_UB_31      -0.0286702000
_diffrn_orient_matrix_UB_32      0.0118316000
_diffrn_orient_matrix_UB_33      -0.0350416000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6085
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        29.500
_diffrn_reflns_theta_max         30.446
_diffrn_reflns_theta_min         3.604
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.310
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       block
_exptl_crystal_F_000             643
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.562
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         6085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0630
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0739P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1314
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4176
_reflns_number_total             6085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ce41268g.txt
_cod_data_source_block           am7
_cod_database_code               7211122
_chemical_oxdiff_formula         'C20 H20 N2 Cl Co'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Co1, Mn1}
3. Uiso/Uaniso restraints and constraints
Uanis(Co1) = Uanis(Mn1)
4. Others
 Fixed Sof: Co1(0.42) Mn1(0.08)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C9(H9), C10(H10)
;
_shelxl_version_number           2013-2