Hydrogen bonding and self-assembly in the crystal structures of ferrocenylmethanol derivatives having different phosphorus substituents on the ferrocene unit
Petr Štěpnička; Ivana Císařová; New J. Chem. 26 (2002) 1389–1396; doi:10.1039/b204655p

data_7050943
_publ_section_title
;
 Hydrogen bonding and self-assembly in the crystal structures of
 ferrocenylmethanol derivatives having different phosphorus
 substituents on the ferrocene unit
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              1389
_journal_page_last               1396
_journal_paper_doi               10.1039/b204655p
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C23 H21 Fe O P S'
_chemical_formula_weight         432.28
_chemical_name_systematic
; 
2-(diphenylthiophosphoryl)ferrocenylmethanol
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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.
_cell_angle_beta                 105.749(1)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   8.6792(1)
_cell_length_b                   17.6265(3)
_cell_length_c                   13.2883(2)
_cell_measurement_reflns_used    17834
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     1956.58(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Giacovazzo, 1994)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 0.110
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Enraf KappaCCD'
_diffrn_measurement_method
;
CCD
rotation scans to fill Ewald sphere
(262 frames; 2 deg omega rotation, 70 s exposure each)
;
_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  0.0153
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8689
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    0.969
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.442
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0294
_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^)+(0.0242P)^2^+1.5162P] where 
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                4135
_reflns_number_total             4488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204655p.txt
_cod_data_source_block           ps670
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7050943