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_7110140
_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         'C45 H55 Cl5 Li3 N O7'
_chemical_formula_sum            'C45 H55 Cl5 Li3 N O7'
_chemical_formula_weight         919.97
_chemical_name_common            'Compound X'
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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             2009-06-05T10:08:26-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                89.201(2)
_cell_angle_beta                 87.934(2)
_cell_angle_gamma                70.5530(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8010(2)
_cell_length_b                   13.9220(3)
_cell_length_c                   18.4310(3)
_cell_measurement_reflns_used    43098
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.513
_cell_volume                     2369.88(8)
_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)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_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      0.0445998
_diffrn_orient_matrix_UB_12      -0.0566843
_diffrn_orient_matrix_UB_13      0.0347289
_diffrn_orient_matrix_UB_21      -0.0951418
_diffrn_orient_matrix_UB_22      0.0155418
_diffrn_orient_matrix_UB_23      0.0270475
_diffrn_orient_matrix_UB_31      -0.0260742
_diffrn_orient_matrix_UB_32      -0.0484509
_diffrn_orient_matrix_UB_33      -0.031779
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0372
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31166
_diffrn_reflns_theta_full        27.55
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         4.06
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            White
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.47
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     570
_refine_ls_number_reflns         10697
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0488
_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^)+(0.0523P)^2^+1.7875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1329
_reflns_number_gt                8035
_reflns_number_total             10697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47393g.txt
_cod_data_source_block           Compound_5_k09mgd06
_cod_database_code               7110140