Synthesis and characterisation of magnesium complexes containing sterically demanding N,N'-bis(aryl)amidinate ligands.
Moxey, Graeme J.; Ortu, Fabrizio; Goldney Sidley, Leon; Strandberg, Helen N.; Blake, Alexander J.; Lewis, William; Kays, Deborah L.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 4838–4846; doi:10.1039/c3dt53234h

data_7028691
_publ_section_title
;
 Synthesis and characterisation of magnesium complexes containing
 sterically demanding N,N'-bis(aryl)amidinate ligands.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4838
_journal_page_last               4846
_journal_paper_doi               10.1039/c3dt53234h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C27 H32 N2'
_chemical_formula_sum            'C27 H32 N2'
_chemical_formula_weight         384.54
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601)
;
_cell_angle_alpha                90
_cell_angle_beta                 127.226(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.799(3)
_cell_length_b                   8.4747(5)
_cell_length_c                   23.577(2)
_cell_measurement_reflns_used    12328
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      74.2560
_cell_measurement_theta_min      3.8790
_cell_volume                     4422.8(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard, H. Puschmann, in preparation (2013)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.9927
_diffrn_measured_fraction_theta_max 0.9760
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'SuperNova Cu'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0028008000
_diffrn_orient_matrix_UB_12      -0.0326365000
_diffrn_orient_matrix_UB_13      -0.0622807000
_diffrn_orient_matrix_UB_21      -0.0693781000
_diffrn_orient_matrix_UB_22      -0.0145217000
_diffrn_orient_matrix_UB_23      -0.0511894000
_diffrn_orient_matrix_UB_31      -0.0052342000
_diffrn_orient_matrix_UB_32      0.1782371000
_diffrn_orient_matrix_UB_33      -0.0151996000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0862
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            36846
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.799
_diffrn_reflns_theta_min         3.921
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_exptl_absorpt_coefficient_mu    0.505
_exptl_absorpt_correction_T_max  1.281
_exptl_absorpt_correction_T_min  0.928
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.4003
_exptl_crystal_size_mid          0.2099
_exptl_crystal_size_min          0.1085
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.241
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4438
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0826
_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^)+(0.1494P)^2^+2.8507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2253
_refine_ls_wR_factor_ref         0.2510
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3245
_reflns_number_total             4438
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3dt53234h.txt
_cod_data_source_block           nhschb
_cod_original_cell_volume        4422.8(10)
_cod_database_code               7028691
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C27 H32 N2'
_chemical_oxdiff_usercomment
'NHSCHB #9185 IN FOMBLIN FILM ON MICROMOUNT FOR HS/DLK'
_reflns_odcompleteness_completeness 99.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-H2 \\sim N1-H1
 with sigma of 0.02
3. Others
 Fixed Sof: H2(0.5) H1(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C7(H7), C23(H23), C12(H12), C14(H14), C21(H21), C5(H5)
4.b Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C9(H9A,H9B,H9C), C26(H26A,H26B,H26C), C15(H15A,H15B,
 H15C), C18(H18A,H18B,H18C), C25(H25A,H25B,H25C), C17(H17A,H17B,H17C), C27(H27A,
 H27B,H27C)
;