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_7033019
_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         '0.5(C39 H62 K N4 O2 P)'
_chemical_formula_sum            'C19.5 H31 K0.5 N2 O P0.5'
_chemical_formula_weight         344.50
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    Moisture-sensitive
_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
_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                74.814(5)
_cell_angle_beta                 79.099(5)
_cell_angle_gamma                84.049(5)
_cell_formula_units_Z            4
_cell_length_a                   9.742(2)
_cell_length_b                   10.616(2)
_cell_length_c                   19.454(5)
_cell_measurement_reflns_used    9755
_cell_measurement_temperature    90
_cell_measurement_theta_max      30.31
_cell_measurement_theta_min      2.58
_cell_volume                     1903.5(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.966
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0302
_diffrn_reflns_av_unetI/netI     0.0353
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39455
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.544
_diffrn_reflns_theta_min         1.991
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.220
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.202
_exptl_crystal_description       Prism
_exptl_crystal_F_000             748
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.390
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         11257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.207
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0625
_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^)+5.7861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1580
_refine_ls_wR_factor_ref         0.1637
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9244
_reflns_number_total             11257
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt03136a2.cif
_cod_data_source_block           mo_mf941_0m
_cod_depositor_comments
'Adding full bibliography for 7033017--7033020.cif.'
_cod_original_cell_volume        1903.6(8)
_cod_original_formula_sum        'C19.50 H31 K0.50 N2 O P0.50'
_cod_database_code               7033019
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.935
_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:
 C18(H18), C21(H21), C15(H15), C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C5(H5a,H5b), C33(H33a,H33b), C32(H32a,H32b), C4(H4a,H4b),
 C35(H35a,H35b), C37(H37a,H37b), C36(H36a,H36b), C39(H39a,H39b), C34(H34a,H34b),
  C38(H38a,H38b)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C29(H29), C11(H11), C28(H28), C27(H27)
2.d Idealised Me refined as rotating group:
 C23(H23a,H23b,H23c), C31(H31a,H31b,H31c), C9(H9a,H9b,H9c), C20(H20a,H20b,
 H20c), C17(H17a,H17b,H17c), C16(H16a,H16b,H16c), C22(H22a,H22b,H22c), C26(H26a,
 H26b,H26c), C19(H19a,H19b,H19c), C10(H10a,H10b,H10c)
;
_olex2_submission_special_instructions 'No special instructions were received'