Functionalization and Isoreticulation in a Series of Metal-Organic Frameworks Derived from Pyridinecarboxylates.
Pachfule, Pradip; Garai, Bikash; Banerjee, Rahul; Inorganic chemistry 55 (2016) 7200–7205; doi:10.1021/acs.inorgchem.6b00758

data_4347903
_publ_contact_author
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Dr. Rahul Banerjee

Scientist
Physical/Materials Chemistry Division  
National Chemical Laboratory
Dr. Homi Bhaba Road
Pune 411008, India

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_publ_section_title
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 Functionalization and Isoreticulation in a Series of Metal-Organic
 Frameworks Derived from Pyridinecarboxylates.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7200
_journal_page_last               7205
_journal_paper_doi               10.1021/acs.inorgchem.6b00758
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C16 H9 Co F2 N2 O4, C3 H6 N O'
_chemical_formula_sum            'C19 H15 Co F2 N3 O5'
_chemical_formula_weight         462.27
_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'
_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                 104.070(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7353(5)
_cell_length_b                   17.7435(7)
_cell_length_c                   11.7645(6)
_cell_measurement_reflns_used    4763
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.1045
_cell_measurement_theta_min      3.1102
_cell_volume                     1971.21(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_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      293
_diffrn_detector_area_resol_mean 16.1640
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measurement_details
;
  1 omega  -83.00  -40.00   1.0000   19.4800
omega____ theta____ kappa____ phi______ frames
    -      -18.6966  -57.0000    0.0000 43

  2 omega  -25.00    2.00   1.0000   19.4800
omega____ theta____ kappa____ phi______ frames
    -      -18.6966   57.0000 -150.0000 27

  3 omega  -33.00   -6.00   1.0000   19.4800
omega____ theta____ kappa____ phi______ frames
    -      -18.6966  -57.0000 -150.0000 27

  4 omega  -50.00   25.00   1.0000   19.4800
omega____ theta____ kappa____ phi______ frames
    -       18.6966  -57.0000   60.0000 75

  5 omega  -52.00   57.00   1.0000   19.4800
omega____ theta____ kappa____ phi______ frames
    -       18.6966  -19.0000  120.0000 109
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0519404000
_diffrn_orient_matrix_UB_12      -0.0211919000
_diffrn_orient_matrix_UB_13      -0.0399264000
_diffrn_orient_matrix_UB_21      0.0198132000
_diffrn_orient_matrix_UB_22      -0.0326596000
_diffrn_orient_matrix_UB_23      0.0348792000
_diffrn_orient_matrix_UB_31      -0.0504899000
_diffrn_orient_matrix_UB_32      0.0090315000
_diffrn_orient_matrix_UB_33      0.0324437000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0187
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            10781
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         3.15
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.917
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.381
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4402
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0529P)^2^+1.8499P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1103
_refine_ls_wR_factor_ref         0.1189
_reflns_number_gt                3482
_reflns_number_total             4402
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00758_si_002.cif
_cod_data_source_block           Co-FPAA-1
_cod_original_cell_volume        1971.20(16)
_cod_database_code               4347903
_reflns_odcompleteness_completeness 95.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H1A,H1B} of C1, H2 of C2, H13 of C13, H15 of C15, H16 of C16, H17 of C17,
  H18 of C18, H6 of C6, H9 of C9, H22 of C22, H23 of C23
 At 1.5 times of:
  {H3A,H3B,H3C} of C3
2. Others
 Fixed Sof: F24(0.5) F25(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C9(H9), C13(H13), C15(H15), C16(H16), C17(H17), C18(H18),
 C22(H22), C23(H23)
3.b X=CH2 refined with riding coordinates:
 C1(H1A,H1B)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
;