Bicyclic guanidinate compounds of magnesium and their activity as pre-catalysts in the Tishchenko reaction
Benjamin M. Day; Natalie E. Mansfield; Martyn P. Coles; Peter B. Hitchcock; Chem.Commun. 47 (2011) 4995–; doi:10.1039/c0cc04789a

data_7106280
_publ_section_title
;
 Bicyclic guanidinate compounds of magnesium and their activity as
 pre-catalysts in the Tishchenko reaction
;
_journal_name_full               Chem.Commun.
_journal_page_first              4995
_journal_paper_doi               10.1039/c0cc04789a
_journal_volume                  47
_journal_year                    2011
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C22 H40 Br2 Mg2 N6 O3, C4 H8 O'
_chemical_formula_sum            'C26 H48 Br2 Mg2 N6 O4'
_chemical_formula_weight         717.12
_chemical_name_systematic
;
?
;
_space_group_IT_number           52
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      52
_symmetry_space_group_name_Hall  '-P 2n 2bc'
_symmetry_space_group_name_H-M   'P n a n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.2
_audit_creation_date             2009-02-06T10:50:22-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.41340(10)
_cell_length_b                   17.0471(2)
_cell_length_c                   21.1472(3)
_cell_measurement_reflns_used    32311
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.733
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     3393.52(7)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.213291E-1
_diffrn_orient_matrix_UB_12      -0.6636E-3
_diffrn_orient_matrix_UB_13      0.463216E-1
_diffrn_orient_matrix_UB_21      -0.103703
_diffrn_orient_matrix_UB_22      -0.50443E-2
_diffrn_orient_matrix_UB_23      0.94148E-2
_diffrn_orient_matrix_UB_31      0.8709E-2
_diffrn_orient_matrix_UB_32      -0.05844
_diffrn_orient_matrix_UB_33      -0.13386E-2
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            55355
_diffrn_reflns_theta_full        26.7
_diffrn_reflns_theta_max         26.7
_diffrn_reflns_theta_min         3.71
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    2.464
_exptl_absorpt_correction_T_max  0.8272
_exptl_absorpt_correction_T_min  0.5252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.212
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     167
_refine_ls_number_reflns         3552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1271P)^2^+11.1160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.188
_refine_ls_wR_factor_ref         0.2024
_reflns_number_gt                2936
_reflns_number_total             3552
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc04789a.txt
_cod_data_source_block           (2a)-jan709b
_cod_database_code               7106280