Synthesis and applications to catalysis of novel cyclopentadienone iron tricarbonyl complexes.
Del Grosso, Alessandro; Chamberlain, Alexander E.; Clarkson, Guy J.; Wills, Martin; Dalton transactions (Cambridge, England : 2003) 47 (2018) 1451–1470; doi:10.1039/c7dt03250a

data_7045212
_publ_section_title
;
 Synthesis and applications to catalysis of novel cyclopentadienone iron
 tricarbonyl complexes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1451
_journal_page_last               1470
_journal_paper_doi               10.1039/c7dt03250a
_journal_volume                  47
_journal_year                    2018
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C20 H20 Fe O5 Si'
_chemical_formula_sum            'C20 H20 Fe O5 Si'
_chemical_formula_weight         424.30
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-12-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-08-07 deposited with the CCDC.
2017-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.56456(12)
_cell_length_b                   15.9301(3)
_cell_length_c                   19.5077(4)
_cell_measurement_reflns_used    19088
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.0780
_cell_measurement_theta_min      3.2590
_cell_volume                     2040.00(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1417
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -15.00  94.00   1.00   50.00    --   17.41  77.00-150.00  109
  2  \w    -15.00  94.00   1.00   50.00    --   17.41  77.00  90.00  109
  3  \w    -15.00  94.00   1.00   50.00    --   17.41  77.00 -30.00  109
  4  \w    -51.00  58.00   1.00   50.00    --  -18.35  77.00-180.00  109
  5  \w    -25.00  37.00   1.00   50.00    --   17.41 -99.00  90.00   62
  6  \w   -107.00 -57.00   1.00   50.00    --  -18.35-178.00-180.00   50
  7  \w   -107.00 -57.00   1.00   50.00    --  -18.35-178.00 -60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0045449000
_diffrn_orient_matrix_UB_12      0.0175522000
_diffrn_orient_matrix_UB_13      -0.0333896000
_diffrn_orient_matrix_UB_21      0.0184709000
_diffrn_orient_matrix_UB_22      0.0401757000
_diffrn_orient_matrix_UB_23      0.0143788000
_diffrn_orient_matrix_UB_31      0.1063596000
_diffrn_orient_matrix_UB_32      -0.0077100000
_diffrn_orient_matrix_UB_33      -0.0010574000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            38542
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         32.391
_diffrn_reflns_theta_min         2.557
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.825
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90335
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.38
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.305
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 2542 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).

 Flack x =   -0.015(10) by classical fit to all intensities  (Shelx 2014)
             -0.018(4) from 2542 selected quotients (Parsons' method)
 Hooft y: -0.018(3)  Olex2
;
_refine_ls_abs_structure_Flack   -0.018(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         6932
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.1482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0638
_reflns_Friedel_coverage         0.736
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.923
_reflns_number_gt                6379
_reflns_number_total             6932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03250a2.cif
_cod_data_source_block           adg7
_cod_depositor_comments
'Adding full bibliography for 7045212--7045216.cif.'
_cod_database_code               7045212
_chemical_oxdiff_formula         'C20 H20 N2 O3 Fe'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_refinement_description
;

The OH was located in a difference map and refined with a DFIX restraint and given thermal 
ellipsoids Uiso 1.5 times the Uequiv of the parent oxygen.

1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O6-H6A
 0.9 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C6(H6)
3.b Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C5(H5A,H5B)
3.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14)
3.d Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.119
_oxdiff_exptl_absorpt_empirical_full_min 0.926