Syntheses, structures and flexible coordination of sterically demanding di- and "tri"-lithiated methandiides.
Sindlinger, Christian P.; Stasch, Andreas; Dalton transactions (Cambridge, England : 2003) 43 (2014) 14334–14345; doi:10.1039/c4dt01185f

data_7031055
_publ_section_title
;
 Syntheses, structures and flexible coordination of sterically demanding
 di- and &quot;tri&quot;-lithiated methandiides.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14334
_journal_page_last               14345
_journal_paper_doi               10.1039/c4dt01185f
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C63.5 H83.5 Li2 N2 O3.25 P2'
_chemical_formula_weight         1002.64
_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_creation_method           SHELXL-97
_cell_angle_alpha                105.93(3)
_cell_angle_beta                 92.96(3)
_cell_angle_gamma                105.66(3)
_cell_formula_units_Z            4
_cell_length_a                   13.234(3)
_cell_length_b                   22.502(5)
_cell_length_c                   22.674(5)
_cell_measurement_reflns_used    46139
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.97
_cell_measurement_theta_min      1.14
_cell_volume                     6194(3)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'X-Seed (Barbour, 1999)'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.940
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device_type  'ADSC quantum 210r'
_diffrn_measurement_method       '\f scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_source         'Australian Synchrotron'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.71071
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            92325
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         1.14
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.9977
_exptl_absorpt_correction_T_min  0.9955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2162
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         0.802
_refine_diff_density_min         -0.498
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.0145(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1278
_refine_ls_number_reflns         24125
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0803P)^2^+4.5821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                19973
_reflns_number_total             24125
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01185f2.cif
_cod_data_source_block           compound5
_cod_depositor_comments
'Adding full bibliography for 7031052--7031060.cif.'
_cod_original_cell_volume        6194(2)
_cod_original_formula_sum        'C63.50 H83.50 Li2 N2 O3.25 P2'
_cod_database_code               7031055