Unprecedented participation of a four-coordinate hydrogen atom in the cubane core of lithium and sodium phenolates
David M. Cousins; Matthew G. Davidson; Daniel Garcia-Vivo; Chem.Commun. 49 (2013) 11809–; doi:10.1039/c3cc47393g

data_7110138
_publ_section_title
;
 Unprecedented participation of a four-coordinate hydrogen atom in the
 cubane core of lithium and sodium phenolates
;
_journal_name_full               Chem.Commun.
_journal_page_first              11809
_journal_paper_doi               10.1039/c3cc47393g
_journal_volume                  49
_journal_year                    2013
_chemical_formula_moiety         'C70 H92 Li6 N2 O10, 2(C4 H8 O)'
_chemical_formula_sum            'C78 H108 Li6 N2 O12'
_chemical_formula_weight         1307.3634
_chemical_name_common            k08mgd02
_chemical_name_systematic
;
?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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             2010-01-07T15:04:43-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 89.79
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8870(2)
_cell_length_b                   13.0390(2)
_cell_length_c                   21.4410(3)
_cell_measurement_reflns_used    109828
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.513
_cell_volume                     3602.78(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_orient_matrix_type       'by Bruker AXS Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0072363
_diffrn_orient_matrix_UB_12      -0.0245949
_diffrn_orient_matrix_UB_13      -0.0439462
_diffrn_orient_matrix_UB_21      -0.0229693
_diffrn_orient_matrix_UB_22      -0.0686569
_diffrn_orient_matrix_UB_23      0.0156132
_diffrn_orient_matrix_UB_31      -0.0737666
_diffrn_orient_matrix_UB_32      0.0237343
_diffrn_orient_matrix_UB_33      -0.0003735
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            63006
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    0.078
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.996
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     589
_refine_ls_number_reflns         8233
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.103
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.098
_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^)+(0.0870P)^2^+7.4704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2448
_refine_ls_wR_factor_ref         0.2525
_reflns_number_gt                7010
_reflns_number_total             8233
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47393g.txt
_cod_data_source_block           Compound_3_k08mgd02
_cod_database_code               7110138