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_7211125
_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 Co N O5'
_chemical_formula_sum            'C13 H9 Co N O5'
_chemical_formula_weight         318.14
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           74
_symmetry_cell_setting           orthorhombic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.2841(15)
_cell_length_b                   7.1837(7)
_cell_length_c                   9.2835(9)
_cell_measurement_reflns_used    1251
_cell_measurement_temperature    566(2)
_cell_measurement_theta_max      70.21
_cell_measurement_theta_min      4.58
_cell_volume                     1286.1(2)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      566(2)
_diffrn_detector_area_resol_mean 10.2833
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1072
_diffrn_reflns_av_sigmaI/netI    0.0579
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2249
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         70.40
_diffrn_reflns_theta_min         4.59
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    10.658
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.90
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSPACK(CrysAlis, Oxford Diffraction)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.610
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         660
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0642
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0292P)^2^+11.6842P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                529
_reflns_number_total             660
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41268g.txt
_cod_data_source_block           am5
_cod_original_sg_symbol_H-M      Imma
_cod_database_code               7211125