Unusual ladder-like supramolecular arrangement by cooperative effect of bifurcated O‒HO hydrogen bonding in crystals of racemic 4-ferrocenylbutan-1,2-diol
Michael Schmittel; Mukul Lal; Marc Schlosser; Hans-Jörg Deiseroth; CrystEngComm 5 (2003) 294–299; doi:10.1039/b304427k

data_7204675
_publ_section_title
;
 Unusual ladder-like supramolecular arrangement by cooperative effect
 of bifurcated O--HO hydrogen bonding in crystals of racemic
 4-ferrocenylbutan-1,2-diol
;
_journal_issue                   50
_journal_name_full               CrystEngComm
_journal_page_first              294
_journal_page_last               299
_journal_paper_doi               10.1039/b304427k
_journal_volume                  5
_journal_year                    2003
_chemical_formula_moiety         C14H18FeO2
_chemical_formula_sum            'C14 H18 Fe O2'
_chemical_formula_weight         274.13
_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                90.00
_cell_angle_beta                 97.460(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2583(10)
_cell_length_b                   9.7626(8)
_cell_length_c                   8.2940(5)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      31.6
_cell_measurement_theta_min      3.25
_cell_volume                     1225.02(15)
_computing_cell_refinement       'CELL/SELECT (STOE IPDS-Software, 1999)'
_computing_data_collection       'EXPOSE (STOE IPDS-Software, 1999)'
_computing_data_reduction        'X-RED (STOE, 1999)'
_computing_molecular_graphics    'DIAMOND 2.1 (Crystal Impact, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       '170 exposures, \D\f=1.3\%'
_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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0216
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17434
_diffrn_reflns_theta_full        31.65
_diffrn_reflns_theta_max         31.65
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_T_max  0.8898
_exptl_absorpt_correction_T_min  0.6787
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.414
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.059
_refine_ls_extinction_coef       0.0039(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         3912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0401P)^2^+0.2061P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0697
_reflns_number_gt                3211
_reflns_number_total             3912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b304427k.txt
_cod_data_source_block           C14H18FeO2
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7204675