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_4330829
_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_moiety         'C3 Ca H19 N O13.50 P3 '
_chemical_formula_sum            'C3 H19 Ca N O13.5 P3'
_chemical_formula_weight         418.18
_chemical_name_systematic
;
Calcium (amino-tris(methylenephosphonate)) hydrate(1/1/4.5)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.0
_cell_angle_beta                 90.655(1)
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   11.3382(5)
_cell_length_b                   8.4555(4)
_cell_length_c                   15.5254(7)
_cell_measurement_reflns_used    7287
_cell_measurement_temperature    173
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      1.50
_cell_volume                     1488.33(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT/NRCVAX DATRD2'
_computing_molecular_graphics    NRCVAX
_computing_publication_material  'NRCVAX TABLES Jan 94 Version'
_computing_structure_refinement  'NRCVAX LSTSQ'
_computing_structure_solution    'NRCVAX SOLVER'
_diffrn_ambient_temperature      173
_diffrn_measurement_device       'Bruker SMART 1K'
_diffrn_measurement_method       'Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'xray tube'
_diffrn_radiation_type           'Molybdenum K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19990
_diffrn_reflns_theta_max         29.95
_diffrn_reflns_theta_min         0.00
_exptl_absorpt_coefficient_mu    0.81
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  1.0000
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_F_000             870.78
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         6.60
_refine_diff_density_min         -5.70
_refine_ls_goodness_of_fit_obs   1.54
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         4274
_refine_ls_R_factor_all          0.036
_refine_ls_R_factor_obs          0.035
_refine_ls_shift/esd_max         0.001
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     1/(\s2^(F)+0.0002F2^)
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.040
_refine_ls_wR_factor_obs         0.040
_reflns_number_observed          3441
_reflns_number_total             4283
_reflns_observed_criterion       'Inet > 2.5\s(Inet)'
_cod_data_source_file            ic301192y_si_002_2.cif
_cod_data_source_block           CaAMP_4.5H2O_new_labels_P21n
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C3 Ca H19 N O13.50 P3 '
_cod_database_code               4330829