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_4347660
_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         'C36 H56 Fe2 N6 P2'
_chemical_formula_sum            'C36 H56 Fe2 N6 P2'
_chemical_formula_weight         746.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 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                 112.2320(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.5781(11)
_cell_length_b                   10.6543(5)
_cell_length_c                   17.4825(8)
_cell_measurement_reflns_used    8495
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      29.36
_cell_measurement_theta_min      2.30
_cell_volume                     3720.4(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX Duo'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            19671
_diffrn_reflns_theta_full        29.45
_diffrn_reflns_theta_max         29.45
_diffrn_reflns_theta_min         2.04
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS. Bruker Nonius area detector scaling and absorption correction - V2.10, Bruker AXS Inc., Madison, Wisconsin, USA (2003).'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1584
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         5155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0348
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+2.0054P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0872
_reflns_number_gt                3928
_reflns_number_total             5155
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b00443_si_003.cif
_cod_data_source_block           mf953
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4347660
_olex2_refinement_description
;
1. Others
 Fixed U12: Fe1(0) Fe2(0)
 Fixed U23: Fe1(0) Fe2(0)
 Fixed Uiso: H17A(0.039) H17B(0.039) H17C(0.039) H13(0.019) H15(0.019)
 H2(0.018) H8A(0.033) H8B(0.033) H8C(0.033) H6(0.019) H18A(0.038) H18B(0.038)
 H18C(0.038) H7A(0.033) H7B(0.033) H7C(0.033) H11A(0.037) H11B(0.037)
 H11C(0.037) H9(0.02) H12(0.019) H5(0.018) H10A(0.033) H10B(0.033) H10C(0.033)
 H16(0.018) H3(0.021) H4(0.021)
 Fixed X: Fe1(0.5) Fe2(0.5) H17A(0.6881) H17B(0.6399) H17C(0.7026) H13(0.6328)
 H15(0.5604) H2(0.3654) H8A(0.2305) H8B(0.2618) H8C(0.2538) H6(0.3311)
 H18A(0.6327) H18B(0.6369) H18C(0.568) H7A(0.4273) H7B(0.3702) H7C(0.3889)
 H11A(0.2263) H11B(0.2085) H11C(0.2669) H9(0.271) H12(0.5812) H5(0.5303)
 H10A(0.3523) H10B(0.3442) H10C(0.2852) H16(0.5129) H3(0.4174) H4(0.5195)
 Fixed Y: H17A(0.6934) H17B(0.697) H17C(0.6086) H13(0.5193) H15(0.3421) H2(-
 0.1845) H8A(0.0317) H8B(0.1433) H8C(0.0113) H6(-0.0706) H18A(0.6205)
 H18B(0.4736) H18C(0.54) H7A(-0.0033) H7B(-0.0232) H7C(0.1127) H11A(0.1973)
 H11B(0.1745) H11C(0.266) H9(0.002) H12(0.3719) H5(-0.1017) H10A(-0.003)
 H10B(0.142) H10C(0.051) H16(0.1986) H3(-0.3871) H4(-0.3364)
 Fixed Z: Fe1(0.25) Fe2(0.25) H17A(0.558) H17B(0.4648) H17C(0.4934)
 H13(0.3771) H15(0.5298) H2(0.1963) H8A(0.2851) H8B(0.3459) H8C(0.3807)
 H6(0.3246) H18A(0.6298) H18B(0.6329) H18C(0.5864) H7A(0.4335) H7B(0.4673)
 H7C(0.4491) H11A(0.1921) H11B(0.0976) H11C(0.1468) H9(0.1742) H12(0.2797)
 H5(0.4004) H10A(0.1146) H10B(0.0984) H10C(0.0503) H16(0.4277) H3(0.2635)
 H4(0.3891)
;