Linking 31P Magnetic Shielding Tensors to Crystal Structures: Experimental and Theoretical Studies on Metal(II) Aminotris(methylenephosphonates)
Johannes Weber; Gisbert Grossmann; Konstantinos D. Demadis; Nikos Daskalakis; Erica Brendler; Martin Mangstl; Jörn Schmedt auf der Günne; Inorganic Chemistry 51 (2012) 11466–11477; doi:10.1021/ic301192y

data_4330828
_publ_contact_author_address
;Department f\"ur Chemie
Ludwig-Maximilians-Universit\"at M\"unchen
Butenandtstr. 5-13 (Haus D)
D-81377 M\"unchen
Germany
;
_publ_contact_author_email       gunnej@cup.uni-muenchen.de
_publ_contact_author_fax         +49-89-2180-77440
_publ_contact_author_name        'J\"orn Schmedt auf der G\"unne'
_publ_contact_author_phone       +49-89-2810-77433
_publ_section_title
;
 Linking 31P Magnetic Shielding Tensors to Crystal Structures:
 Experimental and Theoretical Studies on Metal(II)
 Aminotris(methylenephosphonates)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11466
_journal_page_last               11477
_journal_paper_doi               10.1021/ic301192y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C3 H10 Ba N O9 P3'
_chemical_formula_weight         434.36
_chemical_name_systematic
;
Barium (amino-tris(methylenephosphonate))
;
_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                101.766(3)
_cell_angle_beta                 95.984(3)
_cell_angle_gamma                107.083(2)
_cell_formula_units_Z            2
_cell_length_a                   7.6382(12)
_cell_length_b                   8.4834(13)
_cell_length_c                   9.1417(14)
_cell_measurement_temperature    293(2)
_cell_volume                     545.74(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.910
_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  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3862
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    4.117
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    2.643
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             416
_exptl_crystal_size_max          .18
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .04
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2468
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0263
_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^)+(0.0484P)^2^+0.1838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                2282
_reflns_number_total             2468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301192y_si_002_1.cif
_cod_data_source_block           BaAMP
_cod_original_formula_sum        'C3 H10 Ba1 N1 O9 P3'
_cod_database_code               4330828