3-D Brick-Wall Polymeric Structure of TMEDA-Supported 1,4-Dilithio-1,3-Butadiene
Zhang, Shaoguang; Zhan, Ming; Zhang, Wen-Xiong; Xi, Zhenfeng; Organometallics 32 (2013) 4020–; doi:10.1021/om400531h

data_4081168
_publ_section_title
;
 3-D Brick-Wall Polymeric Structure of TMEDA-Supported
 1,4-Dilithio-1,3-Butadiene
;
_journal_issue                   14
_journal_name_full               Organometallics
_journal_page_first              4020
_journal_paper_doi               10.1021/om400531h
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C9 H18 Li N'
_chemical_formula_sum            'C9 H18 Li N'
_chemical_formula_weight         147.18
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2013-06-18
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr  9 2013 14:06:00, GUI svn.r4458)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   17.806(3)
_cell_length_b                   17.806(3)
_cell_length_c                   12.312(3)
_cell_measurement_temperature    173(2)
_cell_volume                     3903.6(13)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.722
_diffrn_measured_fraction_theta_max 0.728
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.722
_diffrn_reflns_Laue_measured_fraction_max 0.728
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5593
_diffrn_reflns_point_group_measured_fraction_full 0.722
_diffrn_reflns_point_group_measured_fraction_max 0.728
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.364
_diffrn_reflns_theta_min         3.047
_exptl_absorpt_coefficient_mu    0.056
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.002
_exptl_crystal_description       block
_exptl_crystal_F_000             1312
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.149
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.136
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1449
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1005
_refine_ls_R_factor_gt           0.0795
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1105P)^2^+1.8554P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1883
_refine_ls_wR_factor_ref         0.2048
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1187
_reflns_number_total             1449
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om400531h_si_003.cif
_cod_data_source_block           a
_cod_original_cell_volume        3903.7(14)
_cod_database_code               4081168
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Riding coordinates:
 C5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C6(H6a,H6b), C7(H7a,H7b), C8(H8a,H8b)
2.c Me refined with riding coordinates:
 C1(H1a,H1b,H1c), C2(H2a,H2b,H2c), C9(H9a,H9b,H9c)
;
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.982
_shelx_hkl_checksum              97697
_shelx_res_checksum              9752
_shelxl_version_number           2013-3