Crystal structures of 2-(N,N-dimethylaminoalkyl)ferroceneboronic acids and their diol derivatives. The quest for a B‒N intramolecular bond in the solid state
Norrild, Jens Chr.; Søtofte, Inger; Journal of the Chemical Society, Perkin Transactions 2  (2001) 727–; doi:10.1039/b102377m

data_7213476
_publ_section_title
;
 Crystal structures of 2-(N,N-dimethylaminoalkyl)ferroceneboronic acids
 and their diol derivatives. The quest for a B--N intramolecular bond in
 the solid state
;
_journal_issue                   5
_journal_name_full
'Journal of the Chemical Society, Perkin Transactions 2'
_journal_page_first              727
_journal_paper_doi               10.1039/b102377m
_journal_year                    2001
_chemical_formula_sum            'C13 H18 B Fe N O2'
_chemical_formula_weight         286.94
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           29
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.431(4)
_cell_length_b                   6.1956(12)
_cell_length_c                   20.414(4)
_cell_measurement_temperature    120(2)
_cell_volume                     2710.5(9)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_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  0.1247
_diffrn_reflns_av_sigmaI/netI    0.1783
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            17557
_diffrn_reflns_theta_max         29.71
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.104
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_F_000             1200
_refine_diff_density_max         1.310
_refine_diff_density_min         -0.548
_refine_diff_density_rms         0.123
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.47(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.052
_refine_ls_goodness_of_fit_obs   1.133
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         6844
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_restrained_S_obs      1.133
_refine_ls_R_factor_all          0.1632
_refine_ls_R_factor_obs          0.0788
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0444P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1533
_refine_ls_wR_factor_obs         0.1223
_reflns_number_observed          3866
_reflns_number_total             6844
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b102377msup1.cif
_cod_data_source_block           B102377M-4b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0444P)^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^)+(0.0444P)^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        2710.6(9)
_cod_database_code               7213476