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_4347662
_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         'C22 H36 Co1 Fe1 N2 P2'
_chemical_formula_sum            'C22 H36 Co Fe N2 P2'
_chemical_formula_weight         505.25
_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                90.000
_cell_angle_beta                 98.468(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   9.969(5)
_cell_length_b                   12.244(5)
_cell_length_c                   19.170(5)
_cell_measurement_reflns_used    7347
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.65
_cell_volume                     2314.4(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker DUO APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            18977
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.98
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.492
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6585
_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            black
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5307
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0291P)^2^+0.5898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0751
_reflns_number_gt                3991
_reflns_number_total             5307
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic6b00443_si_004.cif
_cod_data_source_block           mo_mf935_0m
_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               4347662
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.012) H10(0.013) H12A(0.018) H12B(0.018) H12C(0.018)
 H16A(0.025) H16B(0.025) H16C(0.025) H14(0.013) H13A(0.021) H13B(0.021)
 H13C(0.021) H17(0.014) H19A(0.027) H19B(0.027) H19C(0.027) H3(0.015)
 H18A(0.031) H18B(0.031) H18C(0.031) H11(0.012) H7(0.013) H20(0.014) H5(0.012)
 H9(0.017) H4(0.014) H21A(0.027) H21B(0.027) H21C(0.027) H15A(0.029)
 H15B(0.029) H15C(0.029) H8(0.018) H22A(0.024) H22B(0.024) H22C(0.024)
 Fixed X: H2(0.1607) H10(0.4487) H12A(-0.0596) H12B(0.0666) H12C(0.0332)
 H16A(0.2062) H16B(0.2751) H16C(0.1173) H14(0.3069) H13A(0.3201) H13B(0.2709)
 H13C(0.3048) H17(0.1351) H19A(0.3497) H19B(0.2809) H19C(0.2593) H3(0.4019)
 H18A(-0.0599) H18B(0.0057) H18C(0.0264) H11(0.0859) H7(0.1448) H20(0.3897)
 H5(0.4115) H9(0.553) H4(0.5551) H21A(0.3085) H21B(0.258) H21C(0.4138)
 H15A(0.2238) H15B(0.1285) H15C(0.2863) H8(0.3664) H22A(0.3456) H22B(0.4366)
 H22C(0.2809)
 Fixed Y: H2(0.1951) H10(0.2454) H12A(-0.0389) H12B(0.0355) H12C(-0.0622)
 H16A(-0.3047) H16B(-0.3345) H16C(-0.3201) H14(-0.1492) H13A(-0.1629) H13B(-
 0.1397) H13C(-0.0422) H17(0.4515) H19A(0.4715) H19B(0.4921) H19C(0.5753)
 H3(0.2413) H18A(0.4385) H18B(0.555) H18C(0.4717) H11(-0.1871) H7(0.3936)
 H20(0.2938) H5(0.0286) H9(0.3554) H4(0.1378) H21A(0.3598) H21B(0.2425)
 H21C(0.2662) H15A(-0.0762) H15B(-0.1777) H15C(-0.1922) H8(0.4466) H22A(0.1108)
 H22B(0.1123) H22C(0.0885)
 Fixed Z: H2(1.1673) H10(0.9567) H12A(1.1784) H12B(1.2027) H12C(1.2502)
 H16A(1.0998) H16B(1.0339) H16C(1.0259) H14(1.0583) H13A(1.1763) H13B(1.2489)
 H13C(1.2014) H17(0.7803) H19A(0.8475) H19B(0.9147) H19C(0.8519) H3(1.2162)
 H18A(0.8353) H18B(0.8444) H18C(0.9072) H11(1.1713) H7(1.0429) H20(0.847)
 H5(1.054) H9(1.0603) H4(1.1465) H21A(0.7328) H21B(0.7089) H21C(0.7273)
 H15A(0.9469) H15B(0.9304) H15C(0.9387) H8(1.114) H22A(0.8754) H22B(0.8153)
 H22C(0.7971)
;