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_7211123
_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      orthorhombic
_space_group_IT_number           74
_space_group_name_Hall           '-I 2b 2'
_space_group_name_H-M_alt        'I m m a'
_symmetry_space_group_name_Hall  '-I 2b 2'
_symmetry_space_group_name_H-M   'I m m a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.2638(11)
_cell_length_b                   7.1952(5)
_cell_length_c                   9.2847(7)
_cell_measurement_reflns_used    1056
_cell_measurement_temperature    296
_cell_measurement_theta_max      30.2777
_cell_measurement_theta_min      3.0161
_cell_volume                     1286.92(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      296
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9783
_diffrn_measurement_details
;
  1 omega   36.00   94.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       14.1593  178.0000  120.0000 58

  2 omega  -89.00   13.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.0968  -57.0000 -120.0000 102

  3 omega   -3.00   26.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.0968  -99.0000    0.0000 29
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0299154000
_diffrn_orient_matrix_UB_12      -0.0406571000
_diffrn_orient_matrix_UB_13      0.0234653000
_diffrn_orient_matrix_UB_21      0.0202717000
_diffrn_orient_matrix_UB_22      -0.0433986000
_diffrn_orient_matrix_UB_23      0.0602949000
_diffrn_orient_matrix_UB_31      -0.0070225000
_diffrn_orient_matrix_UB_32      0.0479634000
_diffrn_orient_matrix_UB_33      0.0743948000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0553
_diffrn_reflns_av_unetI/netI     0.0614
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            3231
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.345
_diffrn_reflns_theta_min         3.582
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.302
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_density_diffrn    1.639
_exptl_crystal_description       block
_exptl_crystal_F_000             643
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.951
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0407P)^2^+4.1840P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1106
_refine_ls_wR_factor_ref         0.1213
_reflns_Friedel_coverage         0.000
_reflns_number_gt                755
_reflns_number_total             973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ce41268g.txt
_cod_data_source_block           am29
_cod_database_code               7211123
_chemical_oxdiff_formula         'C20 H20 N2 O2 Co'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.02
_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)
Uvol(C3) \\sim Uvol(C4): with sigma of 0.1
4. Others
 Fixed Sof: Co1(0.21) Mn1(0.04)
5.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C8(H8), C9(H9)
;
_shelxl_version_number           2013-2