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_7045214
_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         'C26 H22 Fe O8'
_chemical_formula_sum            'C26 H22 Fe O8'
_chemical_formula_weight         518.28
_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
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.60374(7)
_cell_length_b                   14.16447(11)
_cell_length_c                   19.76246(18)
_cell_measurement_reflns_used    16485
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      77.9410
_cell_measurement_theta_min      3.8270
_cell_volume                     2408.40(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 0.994
_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    5.50    --  -41.46 -77.00   0.00  109
  2  \w    -33.00  66.00   1.00    5.50    --   41.46 -38.00-180.00   99
  3  \w     32.00 109.00   1.00   22.00    --  114.00 -95.00 150.00   77
  4  \w     88.00 178.00   1.00   22.00    --  114.00  45.00 -90.00   90
  5  \w     38.00 116.00   1.00   22.00    --  114.00-111.00 -30.00   78
  6  \w     88.00 178.00   1.00   22.00    --  114.00  45.00   0.00   90
  7  \w     38.00 142.00   1.00   22.00    --  114.00 -30.00 -30.00  104
  8  \w   -114.00 -13.00   1.00    5.50    --  -41.46 -57.00-180.00  101
  9  \w     18.00  97.00   1.00    5.50    --   41.46-125.00  60.00   79
 10  \w     61.00 178.00   1.00   22.00    --  114.00  15.00 150.00  117
 11  \w     86.00 178.00   1.00   22.00    --  114.00  30.00-150.00   92
 12  \w     81.00 178.00   1.00   22.00    --  114.00  77.00 -60.00   97
 13  \w     81.00 178.00   1.00   22.00    --  114.00  77.00  30.00   97
 14  \w   -114.00 -13.00   1.00    5.50    --  -41.46 -57.00  90.00  101
 15  \w   -116.00 -17.00   1.00    5.50    --  -41.46 -38.00-120.00   99
 16  \w     32.00 109.00   1.00   22.00    --  114.00 -95.00  30.00   77
 17  \w     88.00 178.00   1.00   22.00    --  114.00  45.00 150.00   90
 18  \w     38.00 147.00   1.00   22.00    --  114.00 -77.00-150.00  109
;
_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      -0.1421843000
_diffrn_orient_matrix_UB_12      -0.0434544000
_diffrn_orient_matrix_UB_13      0.0356396000
_diffrn_orient_matrix_UB_21      0.0748996000
_diffrn_orient_matrix_UB_22      -0.0985734000
_diffrn_orient_matrix_UB_23      -0.0051311000
_diffrn_orient_matrix_UB_31      0.0790574000
_diffrn_orient_matrix_UB_32      0.0150712000
_diffrn_orient_matrix_UB_33      0.0691087000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0253
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24973
_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         78.204
_diffrn_reflns_theta_min         3.840
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.445
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59672
_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    1.429
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.250
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.043
_refine_ls_abs_structure_details
;
 Flack x determined using 2072 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
Hooft y: -0.0063(13) Shelx 2014
Flack x: -0.008(2)   Olex2

;
_refine_ls_abs_structure_Flack   -0.0076(17)
_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     324
_refine_ls_number_reflns         5094
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0437P)^2^+0.4701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0719
_reflns_Friedel_coverage         0.755
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                5009
_reflns_number_total             5094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03250a2.cif
_cod_data_source_block           adg12
_cod_depositor_comments
'Adding full bibliography for 7045212--7045216.cif.'
_cod_database_code               7045214
_chemical_oxdiff_formula         'C20 H20 N2 O2 Fe'
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;

The OHs were located in a difference map and allowed to refine with 
thermal parameters Uiso 1.5 x times Uequiv of the parent oxygen. 
O7-H7 was refined with a DFIX distance restraint

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
 O7-H7
 0.87 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C4(H4A), C7(H7A)
3.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C19(H19), C20(H20), C21(H21), C22(H22)
3.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              32011
_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 1.429
_oxdiff_exptl_absorpt_empirical_full_min 0.793