Synthesis, Structural Characterization, Gas Sorption and Guest-Exchange Studies of the Lightweight, Porous Metal−Organic Framework α-[Mg3(O2CH)6]
Rood, Jeffrey A.; Noll, Bruce C.; Henderson, Kenneth W.; Inorganic Chemistry 45 (2006) 5521–5528; doi:10.1021/ic060543v

data_4332578
_publ_section_title
;
 Synthesis, Structural Characterization, Gas Sorption and Guest-Exchange
 Studies of the Lightweight, Porous Metal&#x2212;Organic Framework
 \a-[Mg3(O2CH)6]
;
_journal_issue                   14
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5521
_journal_page_last               5528
_journal_paper_doi               10.1021/ic060543v
_journal_volume                  45
_journal_year                    2006
_chemical_compound_source        Synthesized
_chemical_formula_moiety         'C5.67 H5.67 Ba3 N0.33 O12.32'
_chemical_formula_sum            'C5.67 H5.67 Ba3 N0.33 O12.32'
_chemical_formula_weight         687.58
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0497(12)
_cell_length_b                   12.706(2)
_cell_length_c                   15.481(2)
_cell_measurement_reflns_used    7564
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.57
_cell_measurement_theta_min      2.63
_cell_volume                     1386.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker X8-ApexII CCD Diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_sigmaI/netI    0.0159
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28698
_diffrn_reflns_theta_full        31.00
_diffrn_reflns_theta_max         31.00
_diffrn_reflns_theta_min         2.07
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Siemens KFFMO2K-90'
_exptl_absorpt_coefficient_mu    8.488
_exptl_absorpt_correction_T_max  0.5511
_exptl_absorpt_correction_T_min  0.2089
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; Blessing, R.H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G.M. (2004) SADABS, University of G\:ottingen, Germany
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1234
_exptl_crystal_recrystallization_method 'From DMF at 120 C'
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.771
_refine_diff_density_min         -1.125
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         2300
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.193
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0176
_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^)+(0.0171P)^2^+2.3356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0423
_refine_ls_wR_factor_ref         0.0427
_reflns_number_gt                2241
_reflns_number_total             2300
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060543vsup11.cif
_cod_data_source_block           jr15ii_0m
_cod_original_cell_volume        1386.6(4)
_cod_database_code               4332578