Synthesis and structures of complexes with axially chiral isoquinolinyl-naphtholate ligands
Howard, Ruth H.; Alonso-Moreno, Carlos; Broomfield, Lewis M.; Hughes, David L.; Wright, Joseph A.; Bochmann, Manfred; Dalton Transactions  (2009) 8667–8682; doi:10.1039/b907982c

data_7002463
_publ_section_title
;
 Synthesis and structures of complexes with axially chiral
 isoquinolinyl-naphtholate ligands
;
_journal_issue                   40
_journal_name_full               'Dalton Transactions'
_journal_page_first              8667
_journal_page_last               8682
_journal_paper_doi               10.1039/b907982c
_journal_year                    2009
_chemical_formula_moiety         'C108 H112 Mg2 N4 O4, 2(C6 H14)'
_chemical_formula_structural     '[{Mg{L(H)}2}2].C6H14'
_chemical_formula_sum            'C120 H140 Mg2 N4 O4'
_chemical_formula_weight         1750.98
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 109.804(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.690(2)
_cell_length_b                   17.4249(15)
_cell_length_c                   22.9030(18)
_cell_measurement_reflns_used    11123
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.4999
_cell_measurement_theta_min      3.5343
_cell_volume                     11148.0(16)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 2008), PLATON (Spek, 2003), WinGX (Farrugia, 1999)
and enCIFer (Allen <i>et al.</i>, 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>, 1993)'
_diffrn_ambient_temperature      140(2)
_diffrn_detector_area_resol_mean 16.0050
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/CCD'
_diffrn_measurement_method       'Thin slice \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0909
_diffrn_reflns_av_sigmaI/netI    0.1383
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            64046
_diffrn_reflns_theta_full        27.71
_diffrn_reflns_theta_max         27.71
_diffrn_reflns_theta_min         3.54
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.043
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3776
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
The strucuture contains a disorered molecule of isohexane, which
may be also be only partial occupancy. This could not be modelled
in a physically-reasonable manner, and was handled using SQUEEZE.
;
_refine_diff_density_max         0.344
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.835
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         12817
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      0.843
_refine_ls_R_factor_all          0.1505
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0848P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1605
_reflns_number_gt                5533
_reflns_number_total             12817
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b907982c.txt
_cod_data_source_block           14
_cod_original_cell_volume        11148.0(15)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7002463