Synthesis of Iron and Cobalt Complexes of a Ferrocene-Linked Diphosphinoamide Ligand and Characterization of a Weak Iron-Cobalt Interaction.
Pick, Fraser S.; Thompson, John R.; Savard, Didier S.; Leznoff, Daniel B.; Fryzuk, Michael D.; Inorganic chemistry 55 (2016) 4059–4067; doi:10.1021/acs.inorgchem.6b00443

data_4347661
_publ_section_title
;
 Synthesis of Iron and Cobalt Complexes of a Ferrocene-Linked
 Diphosphinoamide Ligand and Characterization of a Weak Iron-Cobalt
 Interaction.
;
_journal_issue                   8
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4059
_journal_page_last               4067
_journal_paper_doi               10.1021/acs.inorgchem.6b00443
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C44 H72 Fe4 N4 P4'
_chemical_formula_sum            'C44 H72 Fe4 N4 P4'
_chemical_formula_weight         1004.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.112(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.3912(8)
_cell_length_b                   12.2273(10)
_cell_length_c                   19.1171(15)
_cell_measurement_reflns_used    8086
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.58
_cell_volume                     2415.1(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Apex-II CCD'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            21051
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         1.98
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.344
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_meas      'not meassured'
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.140
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.060
_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     253
_refine_ls_number_reflns         5580
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+1.0997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0634
_reflns_number_gt                4925
_reflns_number_total             5580
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b00443_si_002.cif
_cod_data_source_block           mo_mf922_0m
_cod_database_code               4347661
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H20(0.019) H22A(0.033) H22B(0.033) H22C(0.033) H21A(0.031)
 H21B(0.031) H21C(0.031) H9(0.022) H14(0.017) H2(0.016) H3(0.019) H17(0.02)
 H10(0.018) H18A(0.033) H18B(0.033) H18C(0.033) H7(0.02) H4(0.02) H5(0.017)
 H16A(0.03) H16B(0.03) H16C(0.03) H11(0.02) H15A(0.029) H15B(0.029) H15C(0.029)
 H13A(0.036) H13B(0.036) H13C(0.036) H12A(0.035) H12B(0.035) H12C(0.035)
 H19A(0.039) H19B(0.039) H19C(0.039) H8(0.024)
 Fixed X: H20(0.614) H22A(0.7066) H22B(0.6044) H22C(0.7525) H21A(0.6458)
 H21B(0.7145) H21C(0.5665) H9(0.4415) H14(1.0995) H2(0.5697) H3(0.4308)
 H17(0.8665) H10(0.5419) H18A(0.6599) H18B(0.7497) H18C(0.7222) H7(0.8322)
 H4(0.5775) H5(0.808) H16A(1.3244) H16B(1.2624) H16C(1.3029) H11(1.3333)
 H15A(0.9556) H15B(1.0713) H15C(1.0312) H13A(1.2675) H13B(1.1709) H13C(1.3205)
 H12A(1.2232) H12B(1.293) H12C(1.1435) H19A(1.0474) H19B(0.9623) H19C(0.9894)
 H8(0.6198)
 Fixed Y: H20(0.7095) H22A(0.6489) H22B(0.7403) H22C(0.7682) H21A(0.8919)
 H21B(0.9192) H21C(0.8912) H9(0.6221) H14(0.829) H2(0.9595) H3(0.854)
 H17(0.5609) H10(0.7443) H18A(0.5316) H18B(0.4296) H18C(0.5091) H7(0.6036)
 H4(0.7517) H5(0.7941) H16A(0.8558) H16B(0.8827) H16C(0.9778) H11(0.8581)
 H15A(0.9766) H15B(1.0537) H15C(0.9586) H13A(0.9249) H13B(0.8269) H13C(0.8054)
 H12A(0.7088) H12B(0.6708) H12C(0.6924) H19A(0.5746) H19B(0.5355) H19C(0.4561)
 H8(0.5367)
 Fixed Z: H20(0.157) H22A(0.2683) H22B(0.2784) H22C(0.288) H21A(0.1223)
 H21B(0.1973) H21C(0.1876) H9(-0.0524) H14(0.1803) H2(-0.0547) H3(-0.1472)
 H17(0.2149) H10(0.0443) H18A(0.156) H18B(0.1504) H18C(0.0862) H7(-0.052) H4(-
 0.221) H5(-0.1743) H16A(0.1938) H16B(0.2631) H16C(0.2149) H11(0.0725)
 H15A(0.1795) H15B(0.2058) H15C(0.2541) H13A(-0.0414) H13B(-0.055) H13C(-
 0.0462) H12A(0.117) H12B(0.0524) H12C(0.0434) H19A(0.1515) H19B(0.0835)
 H19C(0.1478) H8(-0.1124)
;