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_7050941
_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'
_chemical_formula_weight         400.22
_chemical_name_systematic
; 
rac-2-(diphenylphosphino)ferrocenylmethanol 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.292(1)
_cell_angle_beta                 81.086(1)
_cell_angle_gamma                80.009(1)
_cell_formula_units_Z            2
_cell_length_a                   7.8638(1)
_cell_length_b                   10.1888(2)
_cell_length_c                   12.0270(2)
_cell_measurement_reflns_used    10607
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     937.46(3)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
CCD
rotation scans to fill Ewald sphere    
(327 frames: 2.0 deg omega rotation, 40 s exposure)
;
_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  0.0144
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6999
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         3.31
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4272
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w=1/[\s^2^(Fo^2^)+(0.0403P)^2^+0.4277P] where 
P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0834
_reflns_number_gt                3841
_reflns_number_total             4272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b204655p.txt
_cod_data_source_block           ps662
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050941