Synthesis and characterization of expected and unexpected topologies of homochiral porous metal(II) malate frameworks
Maxim P. Yutkin; Marina S. Zavakhina; Denis G. Samsonenko; Danil N. Dybtsev; Vladimir P. Fedin; Inorganica Chimica Acta 394 (2013) 367–372; doi:10.1016/j.ica.2012.08.012

data_1512758
_publ_section_title
;
 Synthesis and characterization of expected and unexpected topologies of
 homochiral porous metal(II) malate frameworks
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              367
_journal_page_last               372
_journal_paper_doi               10.1016/j.ica.2012.08.012
_journal_volume                  394
_journal_year                    2013
_chemical_formula_structural     '(Ni2 (C10 H8 N2) (C4 H4 O5)2) . 2(H2 O)'
_chemical_formula_sum            'C18 H20 N2 Ni2 O12'
_chemical_formula_weight         573.78
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.186(1)
_cell_length_b                   6.731(1)
_cell_length_c                   7.575(1)
_cell_measurement_reflns_used    3140
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.0
_cell_measurement_theta_min      3.2
_cell_volume                     1131.2(2)
_computing_cell_refinement       'DENZO (Z. Otwinowski & W. Minor, 1997)'
_computing_data_collection       'ADSC Quantum software'
_computing_data_reduction        'HKL2000 (Z. Otwinowski & W. Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Bruker-AXS, 2004)'
_computing_publication_material  'CIFTAB-97 (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1998)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1998)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 19.5
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'ADSC Quantum 210'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  'Double Crystal Monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.85000
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_sigmaI/netI    0.0392
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7245
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.06
_diffrn_reflns_theta_min         3.22
_diffrn_source                   synchrotron
_diffrn_source_type              'PAL 4A MXW Beamline'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.806
_exptl_absorpt_correction_T_max  0.9460
_exptl_absorpt_correction_T_min  0.8960
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Z. Otwinowski & W. Minor, 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.193
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.163
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.10(3)
_refine_ls_extinction_coef       0.069(7)
_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   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2245
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0575
_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^)+(0.1073P)^2^+1.7270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1578
_refine_ls_wR_factor_ref         0.1604
_reflns_number_gt                2139
_reflns_number_total             2245
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ICA-2013-394-367-372-2.cif
_cod_data_source_block           compound2
_cod_database_code               1512758