Probing Structural Changes in a Phosphonate-based Metal‒Organic Framework Exhibiting Reversible Dehydration
Kinnibrugh, Tiffany L.; Ayi, Ayi A.; Bakhmutov, Vladimir I.; Zoń, Jerzy; Clearfield, Abraham; Crystal Growth & Design 13 (2013) 2973–; doi:10.1021/cg400399v

data_4510767
_publ_section_title
;
 Probing Structural Changes in a Phosphonate-based Metal--Organic
 Framework Exhibiting Reversible Dehydration
;
_journal_issue                   7
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              2973
_journal_paper_doi               10.1021/cg400399v
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         '(C12 H6 O18 P6 Zn5), (C0.50 N0.50), 4(O)'
_chemical_formula_sum            'C12.5 H6 N0.5 O22 P6 Zn5'
_chemical_formula_weight         1027.85
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.430(5)
_cell_length_b                   16.155(12)
_cell_length_c                   19.840(11)
_cell_measurement_reflns_used    1240
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      22.4
_cell_measurement_theta_min      2.52
_cell_volume                     2702(3)
_computing_cell_refinement       'SAINT+  <Bruker, 2005)'
_computing_data_collection       'APEX2   (Bruker, 2005)'
_computing_data_reduction        'SAINT+  <Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008b)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008b>'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008b)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008b)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APEX 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  0.2041
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            17603
_diffrn_reflns_theta_full        27.18
_diffrn_reflns_theta_max         27.18
_diffrn_reflns_theta_min         2.52
_exptl_absorpt_coefficient_mu    4.831
_exptl_absorpt_correction_T_max  0.8686
_exptl_absorpt_correction_T_min  0.4604
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (sheldrick, 2008a)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.527
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2002
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.964
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.229
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         1550
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0611
_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^)+(0.0960P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1869
_reflns_number_gt                974
_reflns_number_total             1550
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cg400399v_si_004.cif
_cod_data_source_block           ZNBTPCH3NH4
_cod_depositor_comments
;
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      'I B A M'
_cod_original_formula_sum        'C12.50 H6 N0.50 O22 P6 Zn5'
_cod_database_code               4510767