Cleavage of an aryl carbon-nitrogen bond of a phosphazido iron(II) complex promoted by hydride metathesis.
Ogawa, Takahiko; Suzuki, Tatsuya; Hein, Nicholas M.; Pick, Fraser S.; Fryzuk, Michael D.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 54–57; doi:10.1039/c4dt03136a

data_7033020
_publ_section_title
;
 Cleavage of an aryl carbon-nitrogen bond of a phosphazido iron(II)
 complex promoted by hydride metathesis.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              54
_journal_page_last               57
_journal_paper_doi               10.1039/c4dt03136a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C35 H54 Br Fe N4 O P'
_chemical_formula_sum            'C35 H54 Br Fe N4 O P'
_chemical_formula_weight         713.55
_chemical_name_systematic        '[NpN3]FeBr(THF)'
_chemical_properties_physical
'Air-sensitive, Moisture-sensitive, Oxygen-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2014-07-10
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.27 svn.r2953 for OlexSys, GUI svn.r4855)
;
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   17.547(5)
_cell_length_b                   10.262(5)
_cell_length_c                   20.588(5)
_cell_measurement_reflns_used    4591
_cell_measurement_temperature    90
_cell_measurement_theta_max      23.25
_cell_measurement_theta_min      2.32
_cell_volume                     3707(2)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2008)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.799
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.799
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11758
_diffrn_reflns_point_group_measured_fraction_full 0.755
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         23.333
_diffrn_reflns_theta_min         1.978
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.559
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.5400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.070
_refine_ls_abs_structure_details
;
 Flack x determined using 1506 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5063
_refine_ls_number_restraints     109
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0425P)^2^+1.8763P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.832
_reflns_Friedel_fraction_full    0.708
_reflns_Friedel_fraction_max     0.883
_reflns_number_gt                3951
_reflns_number_total             5063
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03136a2.cif
_cod_data_source_block           mf966test
_cod_depositor_comments
'Adding full bibliography for 7033017--7033020.cif.'
_cod_database_code               7033020
_shelxl_version_number           2014-3
_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. Uiso/Uaniso restraints and constraints
Uanis(C24) = Uanis(C29) = Uanis(C28) = Uanis(C27) = Uanis(C26) = Uanis(C25) =
Uanis(C30) = Uanis(C31)
Uanis(C24A) = Uanis(C29A) = Uanis(C28A) = Uanis(C27A) = Uanis(C26A) =
Uanis(C25A) = Uanis(C31A) = Uanis(C30A)
Uanis(C35) = Uanis(C34) = Uanis(C33) = Uanis(C32)
3. Rigid body (RIGU) restrains
 C24A, C29A, C28A, C27A, C26A, C25A, C31A, C30A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C24, C29, C28, C27, C26, C25, C30, C31
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C24A)=Sof(C29A)=Sof(C28A)=Sof(H28A)=Sof(C27A)=Sof(H27A)=Sof(C26A)=
 Sof(H26A)=Sof(C25A)=1-FVAR(1)
 Sof(C24)=Sof(C25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27)=Sof(C28)=Sof(H28)=
 Sof(C29)=FVAR(1)
 Sof(C30A)=Sof(H30a)=Sof(H30b)=Sof(H30c)=1-FVAR(2)
 Sof(C30)=Sof(H30d)=Sof(H30e)=Sof(H30f)=FVAR(2)
 Sof(C31A)=Sof(H31a)=Sof(H31b)=Sof(H31c)=1-FVAR(3)
 Sof(C31)=Sof(H31d)=Sof(H31e)=Sof(H31f)=FVAR(3)
5.a Ternary CH refined with riding coordinates:
 C8(H8), C18(H18), C21(H21), C15(H15)
5.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C4(H4a,H4b), C35(H35a,H35b), C3(H3a,H3b), C34(H34a,H34b),
 C33(H33a,H33b), C32(H32a,H32b)
5.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C28A(H28A), C27A(H27A), C26A(H26A), C26(H26),
 C27(H27), C28(H28)
5.d Fitted hexagon refined as free rotating group:
 C24A(C29A,C28A,C27A,C26A,C25A), C24(C25,C26,C27,C28,C29)
5.e Idealised Me refined as rotating group:
 C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C16(H16a,H16b,H16c), C9(H9a,H9b,
 H9c), C19(H19a,H19b,H19c), C17(H17a,H17b,H17c), C20(H20a,H20b,H20c), C10(H10a,
 H10b,H10c), C31A(H31a,H31b,H31c), C30A(H30a,H30b,H30c), C30(H30d,H30e,H30f),
 C31(H31d,H31e,H31f)
;
_olex2_submission_original_sample_id mf966
_olex2_submission_special_instructions 'No special instructions were received'