Metal-Ligand Cooperation in H2 Activation with Iron Complexes Bearing Hemilabile Bis(diphenylphosphino)amine Ligands.
Frank, Nicolas; Hanau, Katharina; Langer, Robert; Inorganic chemistry 53 (2014) 11335–11343; doi:10.1021/ic5022164

data_4341252
_publ_section_title
;
 Metal-Ligand Cooperation in H2 Activation with Iron Complexes Bearing
 Hemilabile Bis(diphenylphosphino)amine Ligands.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11335
_journal_page_last               11343
_journal_paper_doi               10.1021/ic5022164
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C72 H63 Fe N3 P6, 0.5(C7 H8)'
_chemical_formula_sum            'C75.5 H67 Fe N3 P6'
_chemical_formula_weight         1257.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.91(3)
_cell_angle_beta                 101.53(3)
_cell_angle_gamma                106.56(3)
_cell_formula_units_Z            2
_cell_length_a                   12.502(3)
_cell_length_b                   14.942(3)
_cell_length_c                   18.299(4)
_cell_measurement_temperature    100(2)
_cell_volume                     3173.2(14)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_sigmaI/netI    0.0776
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29010
_diffrn_reflns_theta_full        26.75
_diffrn_reflns_theta_max         26.75
_diffrn_reflns_theta_min         1.15
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           32
_diffrn_source_power             1.60
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.436
_exptl_absorpt_correction_T_max  0.9530
_exptl_absorpt_correction_T_min  0.8818
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1314
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.850
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     773
_refine_ls_number_reflns         13336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.850
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0358
_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^)+(0.0317P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0658
_refine_ls_wR_factor_ref         0.0727
_reflns_number_gt                8763
_reflns_number_total             13336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5022164_si_003.cif
_cod_data_source_block           nfm11abs
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Numerical' changed to
'numerical' according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4341251--4341253.cif.
;
_cod_original_cell_volume        3173.2(12)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C75.50 H67 Fe N3 P6'
_cod_database_code               4341252