Contribution of Intramolecular NH...O Hydrogen Bonds to Magnesium-Carboxylate Bonds
Taka-aki Okamura; Junko Nakagawa; Inorganic Chemistry 52 (2013) 10812–10824; doi:10.1021/ic400671v

data_4336139
_publ_section_title
;
 Contribution of Intramolecular NH...O Hydrogen Bonds to
 Magnesium-Carboxylate Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10812
_journal_page_last               10824
_journal_paper_doi               10.1021/ic400671v
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C18 H26 N2 Mg O11'
_chemical_formula_sum            'C18 H26 Mg N2 O11'
_chemical_formula_weight         470.72
_chemical_name_systematic
; 
[Mg(O2C-2-CH3CONHC6H4)(H2O)5][O2C-2-CH3CONHC6H4]
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      1
_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_date             'Fri Apr 20 14:45:51 2007'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.399(15)
_cell_angle_beta                 94.054(11)
_cell_angle_gamma                101.219(14)
_cell_formula_units_Z            4
_cell_length_a                   6.954(2)
_cell_length_b                   14.566(7)
_cell_length_c                   22.183(8)
_cell_measurement_reflns_used    6330
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.0
_cell_volume                     2154.7(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_av_sigmaI/netI    0.1112
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15976
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.146
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.237
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1261
_refine_ls_number_reflns         12513
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1480
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1640
_reflns_number_gt                5314
_reflns_number_total             12513
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic400671v_si_002_8.cif
_cod_data_source_block           8
_cod_original_cell_volume        2155.0(15)
_cod_database_code               4336139