Cooperative Binding of Phosphate Anion and a Neutral Nitrogen Donor to Alkaline-Earth Metal Ions. Investigation of Group 2 Metal-Organophosphate Interaction in the Absence and Presence of 1,10-Phenanthroline
Ramaswamy Murugavel; Subramaniam Kuppuswamy; Sören Randoll; Inorganic Chemistry 47 (2008) 6028–6039; doi:10.1021/ic8003239

data_4305336
_publ_contact_author_address
;
Department of Chemistry
Indian Institute of Technology Bombay
Powai
Mumbai
Maharastra
400076
INDIA
;
_publ_contact_author_email       RMV@CHEM.IITB.AC.IN
_publ_contact_author_name        'Ramaswamy Murugavel'
_publ_section_title
;
Cooperative Binding of Phosphate Anion and a Neutral Nitrogen Donor to
Alkaline-Earth Metal Ions. Investigation of Group 2 Metal-Organophosphate
Interaction in the Absence and Presence of 1,10-Phenanthroline
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6028
_journal_page_last               6039
_journal_paper_doi               10.1021/ic8003239
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C51 H72 Ba1 N4 O13 P2'
_chemical_formula_sum            'C102 H136 Ba2 N8 O26 P4'
_chemical_formula_weight         2288.75
_chemical_name_systematic
;
 ?
;
_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'
_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                 105.720(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.0620(11)
_cell_length_b                   15.3816(11)
_cell_length_c                   24.0717(15)
_cell_measurement_reflns_used    17496
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.4041
_cell_measurement_theta_min      2.9501
_cell_volume                     5368.3(7)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega  -69.00  -17.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1908   92.0000 -144.0000    0.0000    0.0000 52

  2 omega  -55.00   -5.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1908   45.0000  120.0000    0.0000    0.0000 50

  3 omega  -19.00   32.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1908   92.0000 -102.0000    0.0000    0.0000 51

  4 omega   19.00   70.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  -92.0000  -35.0000    0.0000    0.0000 51

  5 omega   49.00  101.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596   75.0000  240.0000    0.0000    0.0000 52

  6 omega   49.00  101.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596   75.0000  120.0000    0.0000    0.0000 52

  7 omega    9.00   37.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  -75.0000    0.0000    0.0000    0.0000 28

  8 phi     63.00  121.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   29.6596    0.0000     -        0.0000    0.0000 58

;
_diffrn_measurement_device_type  'OXFORD DIFFRACTIOM X CALIBUR-S'
_diffrn_measurement_method       'omega(w)-q scan'
_diffrn_orient_matrix_UB_11      -0.0235106913
_diffrn_orient_matrix_UB_12      -0.0397991034
_diffrn_orient_matrix_UB_13      -0.0099886213
_diffrn_orient_matrix_UB_21      -0.0392050256
_diffrn_orient_matrix_UB_22      0.0151749957
_diffrn_orient_matrix_UB_23      0.0083694902
_diffrn_orient_matrix_UB_31      -0.0183642712
_diffrn_orient_matrix_UB_32      0.0185433139
_diffrn_orient_matrix_UB_33      -0.0278596232
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            29369
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.687
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         9390
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.090
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+6.3390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0848
_reflns_number_gt                7564
_reflns_number_total             9390
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8003239-file003_1.cif
_cod_data_source_block           newrm106-relabeled
_cod_original_cell_volume        5368.3(6)
_cod_database_code               4305336