Role of Temperature on Framework Dimensionality: Supramolecular Isomers of Zn3(RCOO)8Based Metal Organic Frameworks
Nagarkar, Sanjog S.; Chaudhari, Abhijeet K.; Ghosh, Sujit K.; Crystal Growth & Design 12 (2012) 572–; doi:10.1021/cg201630c

data_4503026
_publ_section_title
;
 Role of Temperature on Framework Dimensionality: Supramolecular Isomers
 of Zn3(RCOO)8Based Metal Organic Frameworks
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              572
_journal_paper_doi               10.1021/cg201630c
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         'C12 H4 O10 Zn1.50, 1(C2 H8 N)'
_chemical_formula_sum            'C14 H12 N O10 Zn1.5'
_chemical_formula_weight         452.30
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 92.474(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   9.426(5)
_cell_length_b                   15.424(5)
_cell_length_c                   17.359(5)
_cell_measurement_temperature    150(2)
_cell_volume                     2521.4(17)
_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, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25095
_diffrn_reflns_theta_full        28.64
_diffrn_reflns_theta_max         28.64
_diffrn_reflns_theta_min         2.53
_exptl_absorpt_coefficient_mu    1.476
_exptl_absorpt_correction_T_max  0.7568
_exptl_absorpt_correction_T_min  0.6658
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'multi-scan absorption correction'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
The SQUEEZE routine of the program PLATON was used
in order to eliminate the contribution of disordered solvents molecules,
thereby a final model based only on the ordered part of the crystal structure
was obtained.

The SQUEEZE routine suggested that
a total potential solvent area volume of 1067.9 Ang^3^[42.3% of cell volume],
and a void electron population of 165 per cell.

Refinement after the SQUEEZE routine gave significantly improved R values.
[R values before SQUEEZE]
R1 = 0.1386 for >2sigma(I) data
R1 = 0.1524, wR2 = 0.4302, GooF = S = 2.0030 for all data
( 6457 data and 0 restraint / 243 parameters)
;
_refine_diff_density_max         1.387
_refine_diff_density_min         -5.154
_refine_diff_density_rms         0.256
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.525
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         6457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.525
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.1038
_refine_ls_shift/su_max          0.148
_refine_ls_shift/su_mean         0.008
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3378
_refine_ls_wR_factor_ref         0.3523
_reflns_number_gt                5245
_reflns_number_total             6457
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg201630c_si_005.cif
_cod_data_source_block           compound3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C14 H12 N O10 Zn1.50'
_cod_database_code               4503026