Investigating Bidentate and Tridentate Carbamoylmethylphosphine Oxide Ligand Interactions with Rare-Earth Elements Using Electrospray Ionization Quadrupole Ion Trap Mass Spectrometry
Matthew C. Crowe; Ramesh N. Kapoor; Francisco Cervantes-Lee; Laszlo Párkányí; Louis Schulte; Keith H. Pannell; Jennifer S. Brodbelt; Inorganic Chemistry 44 (2005) 6415–6424; doi:10.1021/ic0503028

data_4309486
_publ_section_title
;
Investigating Bidentate and Tridentate Carbamoylmethylphosphine Oxide
Ligand Interactions with Rare-Earth Elements Using Electrospray Ionization
Quadrupole Ion Trap Mass Spectrometry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6415
_journal_page_last               6424
_journal_paper_doi               10.1021/ic0503028
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C40 H65 N2 O3 P'
_chemical_formula_weight         652.91
_chemical_name_common            'Carbamoylmethylphosphine Oxide'
_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           SHELXL-97
_cell_angle_alpha                104.155(3)
_cell_angle_beta                 112.198(3)
_cell_angle_gamma                107.304(3)
_cell_formula_units_Z            2
_cell_length_a                   13.251(2)
_cell_length_b                   13.426(2)
_cell_length_c                   13.845(2)
_cell_measurement_reflns_used    99
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      3
_cell_volume                     1992.0(5)
_computing_cell_refinement       'Bruker SMART V5.625, 2001'
_computing_data_collection       'Bruker SMART V5.625, 2001'
_computing_data_reduction        'Bruker SAINT V5.622, 2001'
_computing_molecular_graphics    'Bruker SHELXTL V6.1012, 2000'
_computing_publication_material  'Bruker SHELXTL V6.1012, 2000'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.735
_diffrn_measured_fraction_theta_max 0.735
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0409
_diffrn_reflns_av_sigmaI/netI    0.0573
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23236
_diffrn_reflns_theta_full        28.42
_diffrn_reflns_theta_max         28.42
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.9772
_exptl_absorpt_correction_T_min  0.9671
_exptl_absorpt_correction_type   'multi-scan (SADABS)'
_exptl_absorpt_process_details   'Bruker SADABS program (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         7378
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0688
_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^)+(0.0626P)^2^+0.5328P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1514
_reflns_number_gt                6116
_reflns_number_total             7378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0503028si20050622_122730.cif
_cod_data_source_block           l952rk1m
_cod_original_cell_volume        1992.1(6)
_cod_database_code               4309486