An orthorhombic polymorph of 1-[(ferrocenyl)(hydroxy)methyl]-1,2-dicarba-<i>closo</i>-dodecaborane
Chen, Hongwei; Miao, Jinling; Zhu, Peihua; Wang, Daqi; Nie, Yong; Acta Crystallographica Section E 66 (2010) m22–; doi:10.1107/S1600536809051903

data_2224600
_publ_section_title
;
 An orthorhombic polymorph of
 1-[(ferrocenyl)(hydroxy)methyl]-1,2-dicarba-<i>closo</i>-dodecaborane
;
_journal_coeditor_code           CV2664
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m22
_journal_paper_doi               10.1107/S1600536809051903
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Fe (C5 H5) (C8 H17 B10 O)]'
_chemical_formula_moiety         'C13 H22 B10 Fe O'
_chemical_formula_sum            'C13 H22 B10 Fe O'
_chemical_formula_weight         358.26
_chemical_name_common
;
1-[Ferrocenyl(hydroxy)methyl]-1,2-dicarbadocecaborane(12)
;
_chemical_name_systematic
;
1-[(ferrocenyl)(hydroxy)methyl]-
1,2-dicarba-<i>closo</i>-dodecaborane
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   27.051(2)
_cell_length_b                   8.9682(7)
_cell_length_c                   29.191(3)
_cell_measurement_reflns_used    3704
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.287
_cell_measurement_theta_min      2.579
_cell_volume                     7081.7(11)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.1154
_diffrn_reflns_av_sigmaI/netI    0.1332
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            35277
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.40
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_T_max  0.9430
_exptl_absorpt_correction_T_min  0.8160
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       yellow
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.124
_refine_diff_density_min         -0.447
_refine_ls_abs_structure_details 'Flack (1983), 5617 Friedel pairs'
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     942
_refine_ls_number_reflns         12025
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1521
_refine_ls_R_factor_gt           0.0748
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0599P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1811
_reflns_number_gt                5629
_reflns_number_total             12025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cv2664.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        7081.8(11)
_cod_database_code               2224600
_cod_database_fobs_code          2224600