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_4510766
_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, 2.8(O), 2(H O0.50), 1.2(N)'
_chemical_formula_sum            'C12 H8 N1.2 O21.8 P6 Zn5'
_chemical_formula_weight         1030.47
_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                   8.472(3)
_cell_length_b                   16.208(7)
_cell_length_c                   19.816(8)
_cell_measurement_reflns_used    3630
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.51
_cell_volume                     2721.0(19)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0725
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18543
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    4.797
_exptl_absorpt_correction_T_max  0.7119
_exptl_absorpt_correction_T_min  0.5552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (sheldrick, 2008a)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.515
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2011
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.794
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         1693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0506
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0610P)^2^+0.3844P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                1315
_reflns_number_total             1693
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cg400399v_si_003.cif
_cod_data_source_block           2ndposelem
_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_cell_volume        2721.1(19)
_cod_original_sg_symbol_Hall     ' -I 2 2c'
_cod_original_sg_symbol_H-M      ' I b a m'
_cod_original_formula_sum        'C12 H8 N1.20 O21.80 P6 Zn5'
_cod_database_code               4510766