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_7110141
_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_sum            'C47 H66 Cl5 N Na3 O7.5'
_chemical_formula_weight         1011.23
_chemical_name_common            'Compound 6'
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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      2.4
_audit_creation_date             2012-12-20
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                107.1770(10)
_cell_angle_beta                 90.7680(10)
_cell_angle_gamma                92.202(2)
_cell_formula_units_Z            4
_cell_length_a                   12.8510(3)
_cell_length_b                   20.6590(5)
_cell_length_c                   21.2810(5)
_cell_measurement_reflns_used    91569
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.513
_cell_volume                     5392.1(2)
_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      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.937
_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      -0.0558832
_diffrn_orient_matrix_UB_12      0.0223656
_diffrn_orient_matrix_UB_13      0.0299819
_diffrn_orient_matrix_UB_21      -0.0379657
_diffrn_orient_matrix_UB_22      -0.0449363
_diffrn_orient_matrix_UB_23      -0.0076837
_diffrn_orient_matrix_UB_31      0.0387774
_diffrn_orient_matrix_UB_32      -0.0072436
_diffrn_orient_matrix_UB_33      0.038247
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.164
_diffrn_reflns_av_unetI/netI     0.1271
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            59857
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    0.34
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2132
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.471
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1177
_refine_ls_number_reflns         23305
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.471
_refine_ls_R_factor_all          0.1766
_refine_ls_R_factor_gt           0.1079
_refine_ls_shift/su_max          0.067
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc
[0.00000+1.00000exp(3.00(sin\q/\l)^2^)]/
[\s^2^(Fo^2^)+0.0400+15.3349*P+(0.0797P)^2^+0.0000sin\q/\l]
where P = 0.10000Fo^2^ + 0.90000Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2834
_refine_ls_wR_factor_ref         0.3557
_reflns_number_gt                12240
_reflns_number_total             23305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc47393g.txt
_cod_data_source_block           Compound_6_h10mgd03
_cod_original_sg_symbol_H-M      P-1
_cod_depositor_comments
;

2023-11-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C94 H132 Cl10 N2 Na6 O15'
_cod_original_formula_weight         2022.46
_cod_original_formula_units_Z            2
_cod_database_code               7110141