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_4347907
_publ_contact_author
;

Dr. Rahul Banerjee

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

;
_publ_section_title
;
 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         'C48 H28 Cd3 F6 N6 O12, 2(C3 H7 N O)'
_chemical_formula_sum            'C54 H42 Cd3 F6 N8 O14'
_chemical_formula_weight         1478.19
_chemical_name_common            Cd-FPAA-1
_chemical_name_systematic
; 
 Cd-FPAA-1 
;
_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                 107.758(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.6945(12)
_cell_length_b                   18.576(2)
_cell_length_c                   14.9208(17)
_cell_measurement_reflns_used    7134
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.28
_cell_volume                     2822.9(5)
_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      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.942
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1066
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31786
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.80
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_T_max  0.864
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-58'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.568
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         6617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0572
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+20.5054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1471
_reflns_number_gt                5740
_reflns_number_total             6617
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00758_si_002.cif
_cod_data_source_block           Cd-FPAA-1
_cod_original_cell_volume        2822.9(6)
_cod_database_code               4347907
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H21 of C21, H22 of C22, H23 of C23, H28 of C28, H29 of C29, H30 of C30, H32
  of C32, H39 of C39, H42 of C42, H1 of C1, H3 of C3, H2 of C2, H8 of C8, H6 of
  C6, H17 of C17
 At 1.5 times of:
  {H4A,H4B,H4C} of C4, {H9A,H9B,H9C} of C9
2. Others
 Fixed Sof: F11(0.75) F1(0.25)
3.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C21(H21), C22(H22), C23(H23), C28(H28), C29(H29), C30(H30),
 C32(H32), C39(H39), C42(H42), C1(H1), C8(H8), C2(H2), C3(H3), C6(H6)
3.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C9(H9A,H9B,H9C)
;