Ytterbium and Samarium Bis(diphosphanylamides): Syntheses and Structures of Lanthanide Complexes Having Two {(Ph2P)2N}-Ligands in the Coordination Sphere
Michael T. Gamer; Peter W. Roesky; Inorganic Chemistry 43 (2004) 4903–4906; doi:10.1021/ic049437o

data_4311406
_publ_contact_author
;
      Prof. Dr. Peter Roesky
      Freie Universit\"at Berlin
      Fabeckstr. 34-36
      14195 Berlin
      Bundesrepublik Deutschland
;
_publ_contact_author_email       roesky@chemie.fu-berlin.de
_publ_contact_author_fax         +49/(0)3083852440
_publ_contact_author_phone       +49/(0)3083854004
_publ_section_title
;
 Ytterbium and Samarium Bis(diphosphanylamides): Syntheses and Structures
 of Lanthanide Complexes Having Two {(Ph2P)2N}-Ligands in the Coordination
 Sphere
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4903
_journal_page_last               4906
_journal_paper_doi               10.1021/ic049437o
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C58 H55 N2 P4 Yb'
_chemical_formula_weight         1076.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 93.33(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.916(2)
_cell_length_b                   21.288(4)
_cell_length_c                   21.608(4)
_cell_measurement_temperature    173(2)
_cell_volume                     5012.8(16)
_computing_molecular_graphics    'Diamond 2.1e'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.914
_diffrn_measured_fraction_theta_max 0.914
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'area detector'
_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  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36499
_diffrn_reflns_theta_full        26.99
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    2.033
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             2188
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .12
_exptl_crystal_size_min          .09
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.935
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         9994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.175
_refine_ls_R_factor_all          0.0260
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+4.3748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0647
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                9262
_reflns_number_total             9994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049437osi20040430_090814.cif
_cod_data_source_block           2
_cod_depositor_comments
;

2020-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C116 H110 N4 P8 Yb2'
_cod_original_formula_weight         2153.92
_cod_original_formula_units_Z            2
_cod_original_cell_volume        5012.5(17)
_cod_database_code               4311406