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_4347902
_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.
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_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 F6 Mn3 N6 O12, 2(C3 H7 N O), 2(C0.50 O0.50)'
_chemical_formula_sum            'C55 H42 F6 Mn3 N8 O15'
_chemical_formula_weight         1333.79
_chemical_name_common            Mn-FPAA-1
_chemical_name_systematic        Mn-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                 111.208(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.8336(6)
_cell_length_b                   18.2867(5)
_cell_length_c                   15.1258(16)
_cell_measurement_reflns_used    4326
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.1691
_cell_measurement_theta_min      2.8832
_cell_volume                     2793.6(4)
_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 0.823
_diffrn_measured_fraction_theta_max 0.674
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10141
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.23
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.764
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.873
_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    1.586
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1354
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         5110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+3.1416P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1268
_reflns_number_gt                4115
_reflns_number_total             5110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00758_si_002.cif
_cod_data_source_block           Mn-FPAA-1
_cod_original_cell_volume        2793.6(3)
_cod_database_code               4347902
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H4 of C4, H74 of C74, H69 of C69, H31 of C31, H33 of C33, H36 of C36, H64
  of C64, H59 of C59, H56 of C56, H53 of C53, H51 of C51, H48 of C48, H46 of
  C46, H45 of C45, H41 of C41
 At 1.5 times of:
  {H2A,H2B,H2C} of C2, {H6A,H6B,H6C} of C6
2. Others
 Fixed Sof: F37(0.75) C5(0.5) O5(0.5) F1(0.25)
3.a Aromatic/amide H refined with riding coordinates:
 C31(H31), C33(H33), C36(H36), C41(H41), C45(H45), C46(H46), C48(H48),
 C51(H51), C53(H53), C56(H56), C59(H59), C64(H64), C69(H69), C74(H74), C4(H4)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C6(H6A,H6B,H6C)
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