Mononuclear iron(ii) complexes containing a tripodal and macrocyclic nitrogen ligand: synthesis, reactivity and application in cyclohexane oxidation catalysis.
Ayad, Massinisa; Klein Gebbink, Robertus J. M.; Le Mest, Yves; Schollhammer, Philippe; Le Poul, Nicolas; Pétillon, François Y; Mandon, Dominique; Dalton transactions (Cambridge, England : 2003) 47 (2018) 15596–15612; doi:10.1039/c8dt02952k

data_7047672
_publ_section_title
;
 Mononuclear iron(ii) complexes containing a tripodal and macrocyclic
 nitrogen ligand: synthesis, reactivity and application in cyclohexane
 oxidation catalysis.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15596
_journal_page_last               15612
_journal_paper_doi               10.1039/c8dt02952k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
;
        C74 H58 Fe2 N14 O8, Cl6 Fe2 O, 3(C2 H3 N)
;
_chemical_formula_sum            'C80 H67 Cl6 Fe4 N17 O9'
_chemical_formula_weight         1846.61
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-07-10T20:14:54-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-07-19 deposited with the CCDC.
2018-09-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.800(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.8448(6)
_cell_length_b                   24.3450(14)
_cell_length_c                   13.5498(7)
_cell_measurement_reflns_used    4147
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      24.38
_cell_measurement_theta_min      3.62
_cell_volume                     3961.0(4)
_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
;
        ORTEP3 for Windows (Farrugia, 1997)
        MERCURY  (Bruno et al., 2002)
;
_computing_publication_material
;
        WinGX (Farrugia, 1999)
        PLATON (Spek, 1990-2003)
        enCIFer (Allen et al., 2004)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1992)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.3622
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0045842
_diffrn_orient_matrix_UB_12      0.027878
_diffrn_orient_matrix_UB_13      0.0130575
_diffrn_orient_matrix_UB_21      0.0183405
_diffrn_orient_matrix_UB_22      0.0084107
_diffrn_orient_matrix_UB_23      -0.0412408
_diffrn_orient_matrix_UB_31      -0.0559746
_diffrn_orient_matrix_UB_32      0.0004659
_diffrn_orient_matrix_UB_33      -0.0355857
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1044
_diffrn_reflns_av_unetI/netI     0.1216
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23434
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.31
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rod, axis [1 0 0]'
_exptl_crystal_F_000             1888
_exptl_crystal_recrystallization_method
'from solution in acetonitrile at room temperature,by slow diffusion of diethylether??????????'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.127
_refine_diff_density_min         -0.572
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         8265
_refine_ls_number_restraints     41
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1408
_refine_ls_R_factor_gt           0.0749
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0917P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1736
_refine_ls_wR_factor_ref         0.2199
_reflns_number_gt                4551
_reflns_number_total             8265
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c8dt02952k2.cif
_cod_data_source_block           ma2015-15-c
_cod_depositor_comments
;Adding full bibliography for 7047672--7047674.cif.

The following automatic conversions were performed:

data name '_iucr_refine_instruction_details' was replaced with
'_iucr_refine_instructions_details' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_sg_symbol_Hall     -P2yb
_cod_original_sg_symbol_H-M      P21/m
_cod_database_code               7047672