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_4323945
_publ_section_title
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 Synthesis and Structures of Intramolecularly Base-Coordinated Aryl Group
 15 Compounds
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_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 Bi'
_chemical_formula_sum            'C27 H36 Bi N3'
_chemical_formula_weight         611.57
_chemical_name_systematic
; 
 ? 
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_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                 90.076(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2996(12)
_cell_length_b                   18.445(3)
_cell_length_c                   15.601(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.97
_cell_measurement_theta_min      2.55
_cell_volume                     2676.1(7)
_computing_cell_refinement       'Enraf CAD4 Express'
_computing_data_collection       'Enraf 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  0.1042
_diffrn_reflns_av_sigmaI/netI    0.1151
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11644
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        8.85
_diffrn_standards_interval_time  1800
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.605
_exptl_absorpt_correction_T_max  0.61909
_exptl_absorpt_correction_T_min  0.13519
_exptl_absorpt_correction_type   SHELXA
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_description       plate
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.19
_refine_diff_density_max         2.023
_refine_diff_density_min         -1.342
_refine_diff_density_rms         0.189
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.081
_refine_ls_goodness_of_fit_obs   1.209
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     552
_refine_ls_number_reflns         9388
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.119
_refine_ls_restrained_S_obs      1.202
_refine_ls_R_factor_all          0.1492
_refine_ls_R_factor_obs          0.0783
_refine_ls_shift/esd_max         0.464
_refine_ls_shift/esd_mean        0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+40.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2132
_refine_ls_wR_factor_obs         0.1716
_reflns_number_observed          5409
_reflns_number_total             9397
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic960516c_3.cif
_cod_data_source_block           Compound6
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+40.0000P] 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^)+(0.0650P)^2^+40.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_database_code               4323945