Dimensionality Transformation through Paddlewheel Reconfiguration in a Flexible and Porous Zn-Based Metal-Organic Framework
Kyriakos C. Stylianou; Jeremy Rabone; Samantha Y. Chong; Romain Heck; Jayne Armstrong; Paul V. Wiper; Kim E. Jelfs; Sergey Zlatogorsky; John Bacsa; Alec G. McLennan; Christopher P. Ireland; Yaroslav Z. Khimyak; K. Mark Thomas; Darren Bradshaw; Matthew J. Rosseinsky; Journal of the American Chemical Society 134 (2012) 20466–20478; doi:10.1021/ja308995t

data_4119024
_publ_section_title
;
 Dimensionality Transformation through Paddlewheel Reconfiguration in a
 Flexible and Porous Zn-Based Metal-Organic Framework
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20466
_journal_page_last               20478
_journal_paper_doi               10.1021/ja308995t
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety
;
2(Zn 2+),(C44 H22 O8 4-), 3(H2 O), 2(C4 H8 O2)
;
_chemical_formula_sum            'C50 H50 O16 Zn2'
_chemical_formula_weight         1037.64
_chemical_name_common            RH430
_space_group_IT_number           10
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2y'
_symmetry_space_group_name_H-M   'P 1 2/m 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                 103.078(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   6.8131(19)
_cell_length_b                   15.782(4)
_cell_length_c                   11.155(3)
_cell_measurement_reflns_used    2330
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      2.3
_cell_volume                     1168.3(5)
_computing_cell_refinement       'SAINT v6.45a (Bruker, 2005)'
_computing_data_collection       'SMART v.5.632 (Bruker, 2005)'
_computing_data_reduction        'SAINT v6.45a (Bruker, 2005)'
_computing_molecular_graphics
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_publication_material
;
 OLEX2: a complete structure solution, refinement and analysis program.
 Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Bruker D8 diffractometer with APEX detector'
_diffrn_measurement_method       '\w scans with a narrow frame width'
_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  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0268
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9130
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_T_max  0.8101
_exptl_absorpt_correction_T_min  0.7339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008-1 (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_description       prism
_exptl_crystal_F_000             538
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
 The structure contains highly disordered dioxane
 and water molecules in the solvent accessible voids.
 Since these molecules were so disordered
 and the electron density in the channels
 diffuse, these were modelled using PLATON/SQUEEZE.
 The electron counts correspond to 1 dioxane in
 void 1, and 1 dioxane and 1 H2O in void 2.
;
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     134
_refine_ls_number_reflns         2201
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0446
_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^)+(0.0848P)^2^+0.6514P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1225
_refine_ls_wR_factor_ref         0.1261
_reflns_number_gt                1965
_reflns_number_total             2201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja308995t_si_003.cif
_cod_data_source_block           RH430M
_cod_original_cell_volume        1168.4(6)
_cod_database_code               4119024