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_7106279
_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 Cl2 Mg2 N6 O2'
_chemical_formula_sum            'C22 H40 Cl2 Mg2 N6 O2'
_chemical_formula_weight         540.12
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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      2.3
_audit_creation_date             2006-02-21T11:47:49-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 109.495(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4059(19)
_cell_length_b                   9.8558(14)
_cell_length_c                   18.998(2)
_cell_measurement_reflns_used    156358
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     2719.2(6)
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_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      0.651215E-1
_diffrn_orient_matrix_UB_12      -0.26651E-1
_diffrn_orient_matrix_UB_13      0.75554E-2
_diffrn_orient_matrix_UB_21      0.20327E-1
_diffrn_orient_matrix_UB_22      0.455182E-1
_diffrn_orient_matrix_UB_23      0.499026E-1
_diffrn_orient_matrix_UB_31      -0.93487E-2
_diffrn_orient_matrix_UB_32      -0.866751E-1
_diffrn_orient_matrix_UB_33      0.238836E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1021
_diffrn_reflns_av_unetI/netI     0.0576
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18368
_diffrn_reflns_theta_full        22.97
_diffrn_reflns_theta_max         22.97
_diffrn_reflns_theta_min         3.49
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.316
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     292
_refine_ls_number_reflns         3590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.09
_refine_ls_R_factor_all          0.0929
_refine_ls_R_factor_gt           0.0754
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+6.2126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1909
_refine_ls_wR_factor_ref         0.2047
_reflns_number_gt                2911
_reflns_number_total             3590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc04789a.txt
_cod_data_source_block           (1b)-feb1806
_cod_original_cell_volume        2719.3(6)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7106279