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_4503024
_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           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                95.596(4)
_cell_angle_beta                 97.431(3)
_cell_angle_gamma                97.238(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3167(16)
_cell_length_b                   9.8122(17)
_cell_length_c                   11.596(2)
_cell_measurement_temperature    150(2)
_cell_volume                     1035.8(3)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18291
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    1.796
_exptl_absorpt_correction_T_max  0.8408
_exptl_absorpt_correction_T_min  0.7152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'multi-scan absorption correction'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_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 263.2 Ang^3^[25.4% of cell volume],
and a void electron population of 72 per cell.

Refinement after the SQUEEZE routine gave significantly improved R values.
[R values before SQUEEZE]
R1 = 0.0787 for >2sigma(I) data
R1 = 0.0832, wR2 = 0.2643, GooF = S = 1.1100 for all data
( 4734 data and 0 restraint / 241 parameters)
;
_refine_diff_density_max         1.366
_refine_diff_density_min         -0.844
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.477
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4734
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.477
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1736P)^2^+3.7280P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1171
_reflns_number_gt                4219
_reflns_number_total             4734
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            cg201630c_si_003.cif
_cod_data_source_block           compound1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C14 H12 N O10 Zn1.50'
_cod_database_code               4503024