Synthesis and Structures of Intramolecularly Base-Coordinated Aryl Group 15 Compounds
Smuruthi Kamepalli; Claire J. Carmalt; Robert D. Culp; Alan H. Cowley; Richard A. Jones; Nicholas C. Norman; Inorganic Chemistry 35 (1996) 6179–6183; doi:10.1021/ic960516c

data_4323944
_publ_section_title
;
 Synthesis and Structures of Intramolecularly Base-Coordinated Aryl Group
 15 Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6179
_journal_page_last               6183
_journal_paper_doi               10.1021/ic960516c
_journal_volume                  35
_journal_year                    1996
_chemical_formula_structural     '((C H3)2 N C H2 C6 H4)3 Sb'
_chemical_formula_sum            'C27 H36 N3 Sb'
_chemical_formula_weight         524.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.278(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.288(2)
_cell_length_b                   18.356(4)
_cell_length_c                   15.566(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.19
_cell_volume                     2653.8(9)
_computing_cell_refinement       'CAD4 Express'
_computing_data_collection       'CAD4 Express'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       '2\q-\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0379
_diffrn_reflns_av_sigmaI/netI    0.0811
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6148
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        '0.907 < d < 1.005'
_diffrn_standards_interval_time  1800
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  0.92428
_exptl_absorpt_correction_T_min  0.53565
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.689
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.15(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.033
_refine_ls_goodness_of_fit_obs   1.141
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     574
_refine_ls_number_reflns         5116
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.105
_refine_ls_restrained_S_obs      1.141
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_obs          0.0520
_refine_ls_shift/esd_max         -0.021
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1247
_refine_ls_wR_factor_obs         0.0906
_reflns_number_observed          2785
_reflns_number_total             5133
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960516c_2.cif
_cod_data_source_block           compound5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2654.1(8)
_cod_database_code               4323944