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_7045215
_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         'C17 H24 Fe O5 Si2'
_chemical_formula_sum            'C17 H24 Fe O5 Si2'
_chemical_formula_weight         420.39
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3151 for OlexSys, GUI svn.r4998)
;
_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                   6.72990(5)
_cell_length_b                   16.17780(13)
_cell_length_c                   19.24565(17)
_cell_measurement_reflns_used    8451
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      77.8740
_cell_measurement_theta_min      4.5680
_cell_volume                     2095.37(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_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 10.2833
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega -111.00  -74.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.7109 -135.0000  103.0000 37

  2 omega -116.00  -17.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.7109  -38.0000  -30.0000 99

  3 omega -108.00  -17.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.7109  -38.0000   60.0000 91

  4 omega   -2.00   48.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -       41.7109  -99.0000  -60.0000 50

  5 omega    4.00   80.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -       41.7109  -99.0000 -180.0000 76

  6 omega   55.00   83.00   1.0000    6.5000
omega____ theta____ kappa____ phi______ frames
    -       41.7109  -99.0000  -60.0000 28

  7 omega   62.00   94.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -135.0000  103.0000 32

  8 omega  101.00  178.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   30.0000   90.0000 77

  9 omega   40.00  116.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000  120.0000 76

 10 omega   67.00  170.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   15.0000    0.0000 103

 11 omega   41.00   67.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000  -30.0000 26

 12 omega   77.00  113.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -111.0000  -30.0000 36

 13 omega  139.00  166.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   45.0000  120.0000 27

 14 omega   96.00  124.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000 -135.0000  103.0000 28

 15 omega   32.00  109.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -95.0000 -150.0000 77

 16 omega   88.00  123.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   45.0000  120.0000 35

 17 omega   85.00  174.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000   61.0000 -150.0000 89

 18 omega  110.00  141.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -77.0000  150.0000 31

 19 omega   40.00   82.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -77.0000  150.0000 42

 20 omega   52.00   91.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -30.0000  150.0000 39

 21 omega   51.00   98.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -45.0000   60.0000 47

 22 omega   44.00  140.00   1.0000   26.0000
omega____ theta____ kappa____ phi______ frames
    -      114.0000  -61.0000  -90.0000 96
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0083746000
_diffrn_orient_matrix_UB_12      -0.0681643000
_diffrn_orient_matrix_UB_13      0.0558211000
_diffrn_orient_matrix_UB_21      0.0105468000
_diffrn_orient_matrix_UB_22      0.0665294000
_diffrn_orient_matrix_UB_23      0.0571431000
_diffrn_orient_matrix_UB_31      -0.2285374000
_diffrn_orient_matrix_UB_32      0.0005514000
_diffrn_orient_matrix_UB_33      0.0046648000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0437
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15745
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.019
_diffrn_reflns_theta_min         3.569
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.016
_refine_diff_density_max         0.439
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 1734 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(2)
_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     233
_refine_ls_number_reflns         4436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0480P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.730
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.980
_reflns_number_gt                4330
_reflns_number_total             4436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03250a2.cif
_cod_data_source_block           adg3
_cod_depositor_comments
'Adding full bibliography for 7045212--7045216.cif.'
_cod_database_code               7045215
_chemical_oxdiff_formula         'C20 H20 N2 O2 Fe'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
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.a Ternary CH refined with riding coordinates:
 C4(H4A)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'