An unprecedented mode of ligation for a bridged amido-cyclopentadienide (constrained geometry) ligand; π-olefinic interactions with gallium and indium
Pietryga, Jeffrey M.; Jones, Jamie N.; Mullins, Lucille A.; Wiacek, Robert J.; Cowley, Alan H.; Chemical Communications (Cambridge, United Kingdom)  (2003) 2072–2073; doi:10.1039/b304940j

data_7113585
_publ_section_title
;
 An unprecedented mode of ligation for a bridged amido-cyclopentadienide
 (constrained geometry) ligand; \p-olefinic interactions with gallium and
 indium
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   16
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2072
_journal_page_last               2073
_journal_paper_doi               10.1039/b304940j
_journal_year                    2003
_chemical_formula_sum            'C24 H24 Br3 N3'
_chemical_formula_weight         594.19
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 119.054(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   28.819(5)
_cell_length_b                   10.496(5)
_cell_length_c                   19.591(5)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      60.52
_cell_measurement_theta_min      3.12
_cell_volume                     5180(3)
_computing_data_collection       'Nonius Collect Software'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.880
_diffrn_measured_fraction_theta_max 0.880
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            23863
_diffrn_reflns_theta_full        30.52
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    5.859
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2940
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.111
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.00030(9)
_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   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+2.8028P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1192
_reflns_number_gt                4922
_reflns_number_total             6955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b304940j.txt
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

2018-03-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C60 H60 Br7.50 N7.50'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1485.48
_cod_database_code               7113585