Stabilization of Hypophosphite in the Binding Pocket of a Dinuclear Macrocyclic Complex: Synthesis, Structure, and Properties of [Ni2L(μ-O2PH2)]BPh4 (L = N6S2 Donor Ligand)
Jochen Lach; Alexander Jeremies; Vasile Lozan; Claudia Loose; Torsten Hahn; Jens Kortus; Berthold Kersting; Inorganic Chemistry 51 (2012) 12380–12388; doi:10.1021/ic301710b

data_4331073
_publ_contact_author_address
; Institut fuer Anorganische Chemie
  Universitaet Leipzig, Johannisallee 29
  04103 Leipzig
  Germany
;
_publ_contact_author_email       b.kersting@uni-leipzig.de
_publ_contact_author_fax         '+49/(0)341/973 6199'
_publ_contact_author_name        'Prof. Dr Berthold Kersting'
_publ_contact_author_phone       '+49/(0)341/973 6143'
_publ_section_title
;
 Stabilization of Hypophosphite in the Binding Pocket of a Dinuclear
 Macrocyclic Complex: Synthesis, Structure, and Properties of
 [Ni2L(\m-O2PH2)]BPh4 (L = N6S2 Donor Ligand)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12380
_journal_page_last               12388
_journal_paper_doi               10.1021/ic301710b
_journal_volume                  51
_journal_year                    2012
_chemical_compound_source
;
 Crystals were obtained by recrystallization from MeCN.
;
_chemical_formula_sum            'C64 H89 B N7 Ni2 O2 P S2'
_chemical_formula_weight         1211.74
_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           'manual editing of form.cif'
_cell_angle_alpha                108.48(3)
_cell_angle_beta                 91.90(3)
_cell_angle_gamma                107.61(3)
_cell_formula_units_Z            2
_cell_length_a                   13.179(3)
_cell_length_b                   15.736(3)
_cell_length_c                   16.799(3)
_cell_measurement_temperature    213(2)
_cell_volume                     3117.1(14)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP3 (FARRUGIA)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'BRUKER AXS'
_diffrn_measurement_method       hemisphere
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.1074
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28567
_diffrn_reflns_theta_full        28.35
_diffrn_reflns_theta_max         28.35
_diffrn_reflns_theta_min         1.29
_exptl_absorpt_coefficient_mu    0.745
_exptl_absorpt_correction_T_max  0.8653
_exptl_absorpt_correction_T_min  0.7964
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             1292
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.419
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.878
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     768
_refine_ls_number_reflns         14655
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.887
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0401
_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^)+(0.0535P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0828
_refine_ls_wR_factor_ref         0.1233
_reflns_number_gt                7874
_reflns_number_total             14655
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301710b_si_002.cif
_cod_data_source_block           hpoh
_cod_original_cell_volume        3117.1(11)
_cod_database_code               4331073