Framework reduction and alkali-metal doping of a triply catenating metal-organic framework enhances and then diminishes H2 uptake.
Mulfort, Karen L.; Wilson, Thea M.; Wasielewski, Michael R.; Hupp, Joseph T.; Langmuir : the ACS journal of surfaces and colloids 25 (2009) 503–508; doi:10.1021/la803014k

data_4503031
_publ_contact_author             'Joseph T. Hupp'
_publ_section_title
;
 Framework reduction and alkali-metal doping of a triply catenating
 metal-organic framework enhances and then diminishes H2 uptake.
;
_journal_issue                   1
_journal_name_full
'Langmuir : the ACS journal of surfaces and colloids'
_journal_page_first              503
_journal_page_last               508
_journal_paper_doi               10.1021/la803014k
_journal_volume                  25
_journal_year                    2009
_chemical_formula_sum            'C18.5 H10 N4 O4 Zn'
_chemical_formula_weight         417.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.845(7)
_cell_angle_beta                 72.778(4)
_cell_angle_gamma                88.703(5)
_cell_formula_units_Z            2
_cell_length_a                   7.815(2)
_cell_length_b                   10.746(3)
_cell_length_c                   13.028(5)
_cell_measurement_reflns_used    4437
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.27
_cell_measurement_theta_min      2.17
_cell_volume                     983.8(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.917
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1098
_diffrn_reflns_av_sigmaI/netI    0.1188
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11429
_diffrn_reflns_theta_full        28.46
_diffrn_reflns_theta_max         28.46
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    1.278
_exptl_absorpt_correction_T_max  0.9346
_exptl_absorpt_correction_T_min  0.8658
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   XPREP
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.057
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.028
_platon_squeeze_details          ' ?'
_refine_diff_density_max         2.890
_refine_diff_density_min         -2.994
_refine_diff_density_rms         0.289
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.112
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         4561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.112
_refine_ls_R_factor_all          0.1558
_refine_ls_R_factor_gt           0.1351
_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^)+(0.1250P)^2^+35.9257P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3601
_refine_ls_wR_factor_ref         0.3686
_reflns_number_gt                3341
_reflns_number_total             4561
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            la803014k_si_002.cif
_cod_data_source_block           zn2ndc2dipytz_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C18.50 H10 N4 O4 Zn'
_cod_database_code               4503031