Thermally stable coordinatively unsaturated alkyl complexes resistant to β-hydride elimination: TpiPrM‒CH2CH3 (M = Co, Fe)
Shirasawa, Nobuhiko; Akita, Munetaka; Hikichi, Shiro; Moro-oka, Yoshihiko; Chemical Communications  (1999) 417–; doi:10.1039/a809441a

data_7110435
_publ_section_title
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 Thermally stable coordinatively unsaturated alkyl complexes resistant to
 \b-hydride elimination: TpiPrM--CH2CH3 (M = Co, Fe)
;
_journal_issue                   5
_journal_name_full               'Chemical Communications'
_journal_page_first              417
_journal_paper_doi               10.1039/a809441a
_journal_year                    1999
_chemical_formula_sum            'C31 H51 B N6 Ni O2'
_chemical_formula_weight         609.30
_chemical_name_common            'compound 3c '
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 97.02(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.968(5)
_cell_length_b                   15.820(2)
_cell_length_c                   21.570(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3376.0(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK?Ga
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6368
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         1.60
_exptl_absorpt_coefficient_mu    0.610
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_F_000             1312
_refine_diff_density_max         1.209
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.990
_refine_ls_goodness_of_fit_obs   2.025
_refine_ls_matrix_type           full
_refine_ls_number_parameters     431
_refine_ls_number_reflns         6368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.990
_refine_ls_restrained_S_obs      2.025
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_obs          0.0844
_refine_ls_shift/esd_max         0.080
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[?Gs^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2375
_refine_ls_wR_factor_obs         0.2337
_reflns_number_observed          5974
_reflns_number_total             6368
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            809441asup1.cif
_cod_data_source_block           shelxl2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[?Gs^2^(Fo^2^)+(0.1000P)^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/[?Gs^2^(Fo^2^)+(0.1000P)^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        3376.2(18)
_cod_database_code               7110435