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_7045213
_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         'C40 H34 Fe O8'
_chemical_formula_sum            'C40 H34 Fe O8'
_chemical_formula_weight         698.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-08-07 deposited with the CCDC.
2017-11-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.7335(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.64408(12)
_cell_length_b                   8.04710(9)
_cell_length_c                   21.6608(2)
_cell_measurement_reflns_used    14346
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      77.8010
_cell_measurement_theta_min      4.0400
_cell_volume                     1679.11(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.992
_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   -118.00  -9.00   1.00    5.00    --  -41.46 -77.00-180.00  109
  2  \w    -70.00  32.00   1.00    5.00    --  -41.46  57.00 -60.00  102
  3  \w    -70.00  32.00   1.00    5.00    --  -41.46  57.00-180.00  102
  4  \w     17.00 116.00   1.00    5.00    --   41.46  38.00  60.00   99
  5  \w     -4.00  82.00   1.00    5.00    --   41.46 -99.00  30.00   86
  6  \w     81.00 178.00   1.00   25.00    --  114.00  77.00 -60.00   97
  7  \w     57.00 151.00   1.00   25.00    --  114.00 178.00-150.00   94
  8  \w     32.00 167.00   1.00   25.00    --  114.00 -15.00 120.00  135
  9  \w     86.00 178.00   1.00   25.00    --  114.00  30.00  30.00   92
 10  \w     42.00 143.00   1.00   25.00    --  114.00 -61.00-150.00  101
 11  \w     38.00 116.00   1.00   25.00    --  114.00-111.00-120.00   78
 12  \w     38.00 116.00   1.00   25.00    --  114.00-111.00   0.00   78
 13  \w    100.00 178.00   1.00   25.00    --  114.00 111.00 120.00   78
 14  \w     32.00 109.00   1.00   25.00    --  114.00 -95.00 150.00   77
 15  \w     38.00 116.00   1.00   25.00    --  114.00-111.00 120.00   78
 16  \w     57.00 151.00   1.00   25.00    --  114.00 178.00 150.00   94
 17  \w   -118.00 -14.00   1.00    5.00    --  -41.46 -77.00  60.00  104
 18  \w   -114.00 -13.00   1.00    5.00    --  -41.46 -57.00 -90.00  101
 19  \w      9.00 118.00   1.00    5.00    --   41.46  77.00 150.00  109
 20  \w     17.00 116.00   1.00    5.00    --   41.46  38.00 -90.00   99
 21  \w      9.00 118.00   1.00    5.00    --   41.46  77.00 -60.00  109
 22  \w     85.00 178.00   1.00   25.00    --  114.00  61.00 120.00   93
 23  \w     81.00 178.00   1.00   25.00    --  114.00  77.00  30.00   97
 24  \w     61.00 178.00   1.00   25.00    --  114.00  15.00-120.00  117
 25  \w     81.00 178.00   1.00   25.00    --  114.00  77.00-150.00   97
 26  \w     81.00 178.00   1.00   25.00    --  114.00  77.00 150.00   97
 27  \w     81.00 178.00   1.00   25.00    --  114.00  77.00  60.00   97
 28  \w     81.00 178.00   1.00   25.00    --  114.00  77.00 -30.00   97
 29  \w     85.00 178.00   1.00   25.00    --  114.00  61.00  90.00   93
 30  \w     81.00 178.00   1.00   25.00    --  114.00  77.00-120.00   97
 31  \w     85.00 178.00   1.00   25.00    --  114.00  61.00 -90.00   93
 32  \w     18.00  97.00   1.00    5.00    --   41.46-125.00 -90.00   79
 33  \w      9.00 118.00   1.00    5.00    --   41.46  77.00  30.00  109
 34  \w     13.00 114.00   1.00    5.00    --   41.46  57.00 120.00  101
 35  \w      9.00 118.00   1.00    5.00    --   41.46  77.00-150.00  109
 36  \w     -4.00  82.00   1.00    5.00    --   41.46 -99.00  60.00   86
 37  \w     81.00 124.00   1.00   25.00    --  114.00  77.00-180.00   43
;
_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      -0.0650685000
_diffrn_orient_matrix_UB_12      -0.1318253000
_diffrn_orient_matrix_UB_13      0.0413493000
_diffrn_orient_matrix_UB_21      -0.0163510000
_diffrn_orient_matrix_UB_22      -0.1185124000
_diffrn_orient_matrix_UB_23      -0.0557315000
_diffrn_orient_matrix_UB_31      0.1451621000
_diffrn_orient_matrix_UB_32      -0.0722443000
_diffrn_orient_matrix_UB_33      0.0159878000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34729
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.268
_diffrn_reflns_theta_min         4.086
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.056
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.32477
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       plate
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 2745 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).

Hooft y: -0.0086(19)  Olex2
Flack x: -0.010(2)    Shelx 2014
;
_refine_ls_abs_structure_Flack   -0.010(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         7091
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0577P)^2^+0.3392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0961
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                6587
_reflns_number_total             7091
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03250a2.cif
_cod_data_source_block           adg11
_cod_depositor_comments
'Adding full bibliography for 7045212--7045216.cif.'
_cod_original_cell_volume        1679.12(3)
_cod_database_code               7045213
_reflns_odcompleteness_completeness 99.95
_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
2.a Ternary CH refined with riding coordinates:
 C4(H4), C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B), C26(H26A,H26B), C33(H33A,H33B)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C19(H19), C20(H20), C21(H21),
 C22(H22), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C35(H35), C36(H36),
  C37(H37), C38(H38), C39(H39)
2.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              2675
_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 2.611
_oxdiff_exptl_absorpt_empirical_full_min 0.740