Stepwise construction of a 4-hydroxyphenyl functionalized O,N,N-tridentate ferrocene-containing enaminone: Spectral, analytical and structural studies
Salvador Celedona; Mauricio Fuentealbab; Thierry Roisnelc; Jean-Rene Hamonc; David Carrilloa; Carolina Manzura; Inorganica Chimica Acta 390 (2012) 184–189; doi:10.1016/j.ica.2012.04.028

data_1512418
_publ_section_title
;
 Stepwise construction of a 4-hydroxyphenyl functionalized
 O,N,N-tridentate ferrocene-containing enaminone: Spectral, analytical and
 structural studies
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              184
_journal_page_last               189
_journal_paper_doi               10.1016/j.ica.2012.04.028
_journal_volume                  390
_journal_year                    2012
_chemical_formula_moiety         'C21 H22 Fe N2 O2'
_chemical_formula_sum            'C21 H22 Fe N2 O2'
_chemical_formula_weight         390.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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_date             2011-07-01
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.02.15 svn.r1672, GUI svn.r3494)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 101.185(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.1849(2)
_cell_length_b                   9.72339(18)
_cell_length_c                   20.6783(4)
_cell_measurement_reflns_used    11374
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      29.1264
_cell_measurement_theta_min      2.6402
_cell_volume                     1811.67(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr  6 2011,09:17:13)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr  6 2011,09:17:13)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr  6 2011,09:17:13)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'A short history of SHELX (Sheldrick, 2007)'
_diffrn_ambient_temperature      120.0
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
  1 omega   -4.00   23.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   77.0000  -90.0000 27

  2 omega  -47.00   52.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   77.0000  150.0000 99

  3 omega  -10.00   76.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -       18.5616   77.0000  -60.0000 86

  4 omega   49.00   86.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -       18.5616   77.0000 -120.0000 37

  5 omega  -90.00    8.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -38.0000  120.0000 98

  6 omega  -88.00   12.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -77.0000   30.0000 100

  7 omega  -94.00  -32.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  179.0000  -30.0000 62

  8 omega  -94.00  -32.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  179.0000  150.0000 62

  9 omega  -90.00    8.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -38.0000 -150.0000 98

 10 omega   26.00   84.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -137.0000   40.0000 58

 11 omega  -94.00  -32.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  179.0000  -90.0000 62

 12 omega  -43.00   54.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   38.0000  -60.0000 97

 13 omega  -88.00   12.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -77.0000  120.0000 100

 14 omega  -43.00   54.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   38.0000  150.0000 97

 15 omega   24.00   82.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -134.0000 -104.0000 58

 16 omega   26.00   84.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -137.0000 -139.0000 58

 17 omega  -94.00  -32.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  179.0000  -60.0000 62

 18 omega  -90.00    8.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -35.0000  -59.0000 98

 19 omega  -54.00   92.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -       18.5616    0.0000 -180.0000 146

 20 omega  -11.00   89.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -       18.5616   77.0000 -180.0000 100

 21 omega  -11.00   89.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -       18.5616   77.0000  -30.0000 100

 22 omega   26.00   84.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -137.0000   76.0000 58

 23 omega  -54.00  -29.00   1.0000    9.9800
omega____ theta____ kappa____ phi______ frames
    -       18.5616    0.0000 -150.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0721113000
_diffrn_orient_matrix_UB_12      0.0227190000
_diffrn_orient_matrix_UB_13      0.0148783000
_diffrn_orient_matrix_UB_21      -0.0234276000
_diffrn_orient_matrix_UB_22      0.0693113000
_diffrn_orient_matrix_UB_23      -0.0052020000
_diffrn_orient_matrix_UB_31      -0.0211896000
_diffrn_orient_matrix_UB_32      0.0007121000
_diffrn_orient_matrix_UB_33      0.0312093000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            63872
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.19
_diffrn_reflns_theta_min         2.72
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.10 (release 06-04-2011 CrysAlis171 .NET)
(compiled Apr  6 2011,09:17:13)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4717
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+1.0503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0856
_reflns_number_gt                3573
_reflns_number_total             4717
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-390-184-189-4.cif
_cod_data_source_block           complex4
_cod_original_cell_volume        1811.68(7)
_cod_database_code               1512418