Thermodynamic Study of CO2 Sorption by Polymorphic Microporous MOFs with Open Zn(II) Coordination Sites.
Ahrenholtz, Spencer R.; Landaverde-Alvarado, Carlos; Whiting, Macauley; Lin, Shaoyang; Slebodnick, Carla; Marand, Eva; Morris, Amanda J.; Inorganic chemistry 54 (2015) 4328–4336; doi:10.1021/ic503047y

data_4342804
_publ_section_title
;
 Thermodynamic Study of CO2 Sorption by Polymorphic Microporous MOFs with
 Open Zn(II) Coordination Sites.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4328
_journal_page_last               4336
_journal_paper_doi               10.1021/ic503047y
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'C19 H17 N3 O9 Zn2'
_chemical_formula_sum            'C19 H17 N3 O9 Zn2'
_chemical_formula_weight         562.09
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-02-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.23325(19)
_cell_length_b                   17.4883(3)
_cell_length_c                   20.3322(5)
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.4404
_cell_measurement_theta_min      3.4288
_cell_volume                     4349.85(15)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 16.0122
_diffrn_detector_type            'Oxford Diffraction Eos CCD'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -53.00   39.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753   57.0000   30.0000 92

  2 omega  -92.00    0.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  129.0000  135.0000 92

  3 omega  -50.00   41.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753   38.0000  150.0000 91

  4 omega  -92.00  -64.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -77.0000    0.0000 28

  5 omega  -29.00    2.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -77.0000    0.0000 31

  6 omega -100.00  -34.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.3753  -57.0000 -120.0000 66
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0100747726
_diffrn_orient_matrix_UB_12      -0.0394828178
_diffrn_orient_matrix_UB_13      0.0050990420
_diffrn_orient_matrix_UB_21      0.0042100116
_diffrn_orient_matrix_UB_22      0.0054898401
_diffrn_orient_matrix_UB_23      0.0344580997
_diffrn_orient_matrix_UB_31      -0.0569600317
_diffrn_orient_matrix_UB_32      0.0073892638
_diffrn_orient_matrix_UB_33      0.0016449659
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_av_unetI/netI     0.0341
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37739
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        30.000
_diffrn_reflns_theta_max         30.519
_diffrn_reflns_theta_min         3.529
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_target            Mo
_diffrn_source_type              'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.262
_exptl_absorpt_correction_T_max  0.866
_exptl_absorpt_correction_T_min  0.739
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.717
_exptl_crystal_description       block
_exptl_crystal_F_000             2272
_exptl_crystal_recrystallization_method 'precipated from diethylformamide'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.009
_refine_diff_density_min         -1.117
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     319
_refine_ls_number_reflns         6633
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0492
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+14.3246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1112
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5162
_reflns_number_total             6633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic503047y_si_002.cif
_cod_data_source_block           cs1813
_cod_depositor_comments
'Adding full bibliography for 4342803--4342804.cif.'
_cod_original_cell_volume        4349.85(14)
_cod_database_code               4342804
_chemical_oxdiff_formula         'C19 H16 N3 O9 Zn2'
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
O9A \\sim O9B \\sim C15A \\sim C15B: within 1.7A with sigma of 0.02 and sigma
for terminal atoms of 0.04
3. Others
 Sof(O9B)=Sof(C15B)=Sof(H15B)=1-FVAR(1)
 Sof(O9A)=Sof(C15A)=Sof(H15A)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C18(H18A,H18B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C9(H9), C10(H10), C12(H12), C15A(H15A), C15B(H15B)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C19(H19A,H19B,H19C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 'edit lst'
_olex2_date_sample_submission    '15 Dec 2011'
_olex2_submission_special_instructions 'No special instructions were received'