Regulation of the Hydrolytic Activity of Mg(2+)-Dependent Phosphatase Models by Intramolecular NH···O Hydrogen Bonds.
Okamura, Taka-Aki; Furuya, Ryosuke; Onitsuka, Kiyotaka; Journal of the American Chemical Society 136 (2014) 14639–14641; doi:10.1021/ja509006x

data_4122790
_publ_section_title
;
 Regulation of the Hydrolytic Activity of Mg(2+)-Dependent Phosphatase
 Models by Intramolecular NH&#x00B7;&#x00B7;&#x00B7;O Hydrogen Bonds.
;
_journal_issue                   42
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14639
_journal_page_last               14641
_journal_paper_doi               10.1021/ja509006x
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C108 H158 Mg N4 O24'
_chemical_formula_sum            'C108 H158 Mg N4 O24'
_chemical_formula_weight         1920.68
_chemical_name_systematic
; 
[{(t-BuC6H4)3CCONH](n-BuCONH)C6H3COO}2Mg(H2O)4]-5(dioxane)-2H2O
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2014-08-25
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                91.046(6)
_cell_angle_beta                 93.877(7)
_cell_angle_gamma                98.227(7)
_cell_formula_units_Z            1
_cell_length_a                   11.2149(9)
_cell_length_b                   15.3785(12)
_cell_length_c                   15.9820(11)
_cell_measurement_reflns_used    9980
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.00
_cell_volume                     2720.7(4)
_computing_cell_refinement       'RAPID AUTO (Rigaku, 2006)'
_computing_data_collection       'RAPID AUTO (Rigaku, 2006)'
_computing_data_reduction        'RAPID AUTO (Rigaku, 2006)'
_computing_molecular_graphics    'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID II'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20826
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.000
_diffrn_source
;
 MicroMax-007HF microfocus rotating anode X-ray generator
;
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1038
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     702
_refine_ls_number_reflns         9566
_refine_ls_number_restraints     67
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0714
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+1.4424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1861
_refine_ls_wR_factor_ref         0.1997
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7373
_reflns_number_total             9566
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja509006x_si_002.cif
_cod_data_source_block           Mg-L1-5(dioxane)-2H2O
_cod_depositor_comments
'Adding full bibliography for 4122790--4122793.cif.'
_cod_database_code               4122790
_shelx_estimated_absorpt_t_min   0.974
_shelx_estimated_absorpt_t_max   0.991
_shelxl_version_number           2014/6
_shelx_hkl_checksum              43392