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_7033018
_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         'C31 H47 N4 P'
_chemical_formula_sum            'C31 H47 N4 P'
_chemical_formula_weight         506.70
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_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                68.433(2)
_cell_angle_beta                 80.379(2)
_cell_angle_gamma                83.219(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4137(10)
_cell_length_b                   12.3149(14)
_cell_length_c                   16.0458(19)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    90
_cell_measurement_theta_max      29.687
_cell_measurement_theta_min      2.460
_cell_volume                     1521.5(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32276
_diffrn_reflns_theta_full        29.71
_diffrn_reflns_theta_max         29.71
_diffrn_reflns_theta_min         1.38
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.115
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.7113
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0604 before and 0.0336 after correction. The Ratio of minimum to maximum transmission is 0.9536. The \l/2 correction factor is 0.0015.'
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         8629
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0372
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+0.5686P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                7553
_reflns_number_total             8629
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c4dt03136a2.cif
_cod_data_source_block           mo_mf936_0m
_cod_depositor_comments
'Adding full bibliography for 7033017--7033020.cif.'
_cod_database_code               7033018
_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:
 C21(H21), C18(H18), C8(H8), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b), C3(H3a,H3b), C4(H4a,H4b)
2.c Aromatic/amide H refined with riding coordinates:
 C28(H28), C13(H13), C27(H27), C11(H11), C29(H29), C12(H12)
2.d Idealised Me refined as rotating group:
 C26(H26a,H26b,H26c), C19(H19a,H19b,H19c), C9(H9a,H9b,H9c), C16(H16a,H16b,
 H16c), C20(H20a,H20b,H20c), C31(H31a,H31b,H31c), C17(H17a,H17b,H17c), C23(H23a,
 H23b,H23c), C10(H10a,H10b,H10c), C22(H22a,H22b,H22c)
;
_olex2_submission_special_instructions 'No special instructions were received'