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_1512417
_publ_contact_author_name
;
;
_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         'C19 H16 Fe O3'
_chemical_formula_sum            'C19 H16 Fe O3'
_chemical_formula_weight         348.17
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-09-02
_audit_creation_method
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  Olex2 1.1
  (compiled 2011.09.01 svn.r1953, GUI svn.r3819)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.7943(6)
_cell_length_b                   17.2850(16)
_cell_length_c                   17.4952(5)
_cell_measurement_reflns_used    13120
_cell_measurement_temperature    120
_cell_measurement_theta_max      29.2658
_cell_measurement_theta_min      2.6044
_cell_volume                     2961.8(3)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.38 (release 10-08-2010 CrysAlis171 .NET)
(compiled Aug 10 2010,17:59:35)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.38 (release 10-08-2010 CrysAlis171 .NET)
(compiled Aug 10 2010,17:59:35)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.38 (release 10-08-2010 CrysAlis171 .NET)
(compiled Aug 10 2010,17:59:35)
;
_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, G.M. Sheldrick, Acta Cryst.
2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      120
_diffrn_detector_area_resol_mean 16.1511
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.921
_diffrn_measurement_details
;
  1 omega  -83.00   32.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366    0.0000  -60.0000 230

  2 omega   41.00   80.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -141.0000  176.0000 78

  3 omega  -88.00   12.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -77.0000 -120.0000 200

  4 omega  -94.00  -32.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  179.0000    0.0000 124

  5 omega  -88.00   12.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -77.0000   90.0000 200

  6 omega  -43.00   54.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366   38.0000    0.0000 194

  7 omega  -90.00  -42.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.9366  -38.0000  -90.0000 96

  8 omega   29.00   86.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       18.5616 -141.0000  -55.0000 114
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0109567000
_diffrn_orient_matrix_UB_12      0.0168213000
_diffrn_orient_matrix_UB_13      -0.0364599000
_diffrn_orient_matrix_UB_21      0.0172786000
_diffrn_orient_matrix_UB_22      0.0356027000
_diffrn_orient_matrix_UB_23      0.0176775000
_diffrn_orient_matrix_UB_31      0.0694742000
_diffrn_orient_matrix_UB_32      -0.0115045000
_diffrn_orient_matrix_UB_33      0.0013368000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.1024
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37603
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.2658
_diffrn_reflns_theta_min         2.6044
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84782
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.38 (release 10-08-2010 CrysAlis171 .NET)
(compiled Aug 10 2010,17:59:35)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0281P)^2^+1.9196P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0724
_reflns_number_gt                3210
_reflns_number_total             3744
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2012-390-184-189-3.cif
_cod_data_source_block           complex3
_cod_database_code               1512417