Syntheses of two imidazolate-4-amide-5-imidate linker-based hexagonal metal‒organic frameworks with flexible ethoxy substituent
Mondal, Suvendu Sekhar; Dey, Subarna; Baburin, Igor A.; Kelling, Alexandra; Schilde, Uwe; Seifert, Gotthard; Janiak, Christoph; Holdt, Hans-Jürgen; CrystEngComm 15 (2013) 9394–; doi:10.1039/c3ce41632a

data_7214560
_publ_section_title
;
 Syntheses of two imidazolate-4-amide-5-imidate linker-based hexagonal
 metal--organic frameworks with flexible ethoxy substituent
;
_journal_issue                   45
_journal_name_full               CrystEngComm
_journal_page_first              9394
_journal_paper_doi               10.1039/c3ce41632a
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C7 H8 N4 O3 Zn, 0.5(C3H7O)'
_chemical_formula_sum            'C8.5 H11.5 N4.5 O3.5 Zn'
_chemical_formula_weight         298.09
_chemical_name_systematic
;
 (2-ethoxy-imidazolate-4-amide-5-imidato)-zinc(II) dimethylformamide solvate
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            18
_cell_length_a                   18.0166(5)
_cell_length_b                   18.0166(5)
_cell_length_c                   18.6077(5)
_cell_measurement_reflns_used    32841
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      29.69
_cell_measurement_theta_min      1.70
_cell_volume                     5230.8(2)
_computing_cell_refinement       'X-AREA (Stoe, 2004)'
_computing_data_collection       'X-AREA (Stoe, 2004)'
_computing_data_reduction        'X-RED (Stoe, 2004)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      210(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
 360 frames, exposure time = 4 min
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scan, \d \w = 1.0 deg'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0079
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29403
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.70
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           40
_diffrn_source_power             2.00
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.122
_exptl_absorpt_correction_T_max  0.8281
_exptl_absorpt_correction_T_min  0.6101
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-Red (Stoe, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.00011(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2681
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0236
_refine_ls_R_factor_gt           0.0212
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0316P)^2^+7.6193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0559
_refine_ls_wR_factor_ref         0.0569
_reflns_number_gt                2506
_reflns_number_total             2681
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce41632a.txt
_cod_data_source_block           IFP-9
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7214560