A new anthraquinoid ligand for the iron-catalyzed hydrosilylation of carbonyl compounds at room temperature: new insights and kinetics.
Raya-Barón, Álvaro; Galdeano-Ruano, Carmen P; Oña-Burgos, Pascual; Rodríguez-Diéguez, Antonio; Langer, Robert; López-Ruiz, Rosalía; Romero-González, Roberto; Kuzu, Istemi; Fernández, Ignacio; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7272–7281; doi:10.1039/c8dt01123k

data_7046097
_publ_section_title
;
 A new anthraquinoid ligand for the iron-catalyzed hydrosilylation of
 carbonyl compounds at room temperature: new insights and kinetics.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7272
_journal_page_last               7281
_journal_paper_doi               10.1039/c8dt01123k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C44 H34 Fe N4 O4.50'
_chemical_formula_sum            'C44 H34 Fe N4 O4.5'
_chemical_formula_weight         746.60
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-10-02 deposited with the CCDC.
2018-04-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 115.42(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.547(2)
_cell_length_b                   14.268(1)
_cell_length_c                   17.633(2)
_cell_measurement_reflns_used    12000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      1.5
_cell_volume                     3532.7(7)
_computing_cell_refinement       'IPDS II (Stoe)'
_computing_data_collection       'IPDS II (Stoe)'
_computing_data_reduction        'IPDS II (Stoe)'
_computing_publication_material  'WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
;
 SIR-92 (Altomare, Cascarano, Giacovazzo, Guagliardi, Burla, Polidori,
        Camalli, 1992)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'IPDS II (Stoe)'
_diffrn_measurement_method       'IPDS II (Stoe)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1553
_diffrn_reflns_av_unetI/netI     0.1631
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27765
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.108
_diffrn_reflns_theta_min         1.450
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.480
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-red32/X-area (Stoe)'
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       plates
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.656
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     483
_refine_ls_number_reflns         6908
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.1678
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0694P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1791
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3158
_reflns_number_total             6908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01123k2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7046096--7046097.cif.
;
_cod_original_formula_sum        'C44 H34 Fe N4 O4.50'
_cod_database_code               7046097
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              66107