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_4305340
_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         'C48 H54 Ca1 N4 O9 P2'
_chemical_formula_sum            'C48 H54 Ca N4 O9 P2'
_chemical_formula_weight         932.97
_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                 100.874(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.5565(3)
_cell_length_b                   16.4318(3)
_cell_length_c                   21.6158(4)
_cell_measurement_reflns_used    19121
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.5905
_cell_measurement_theta_min      2.9126
_cell_volume                     4728.63(16)
_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      150(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -56.00   -5.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.0346   45.0000  240.0000    0.0000    0.0000 51

  2 omega  -11.00   43.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.0346   75.0000  120.0000    0.0000    0.0000 54

  3 omega -101.00  -47.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.0346  -75.0000  120.0000    0.0000    0.0000 54

  4 omega  -60.00   -7.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.0346   75.0000  240.0000    0.0000    0.0000 53

  5 omega  -60.00   -8.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.0346   75.0000  120.0000    0.0000    0.0000 52

  6 omega    6.00   57.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  -45.0000  240.0000    0.0000    0.0000 51

  7 omega    8.00   54.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  -75.0000    0.0000    0.0000    0.0000 46

  8 omega  -43.00    7.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  -45.0000  240.0000    0.0000    0.0000 50

  9 omega  -35.00   -4.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  134.0000    1.0000    0.0000    0.0000 31

 10 omega  -43.00  -15.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  -75.0000  240.0000    0.0000    0.0000 28

 11 omega   29.00   57.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  -75.0000  240.0000    0.0000    0.0000 28

 12 omega   48.00   91.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596   75.0000    0.0000    0.0000    0.0000 43

 13 omega  -43.00   12.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.6596  -75.0000    0.0000    0.0000    0.0000 55

;
_diffrn_measurement_device_type  'OXFORD DIFFRACTIOM X CALIBUR-S'
_diffrn_measurement_method       'omega(w)-q scan'
_diffrn_orient_matrix_UB_11      -0.0504261924
_diffrn_orient_matrix_UB_12      -0.0019966781
_diffrn_orient_matrix_UB_13      0.0045562021
_diffrn_orient_matrix_UB_21      -0.0100122578
_diffrn_orient_matrix_UB_22      -0.0315086728
_diffrn_orient_matrix_UB_23      -0.0227733229
_diffrn_orient_matrix_UB_31      0.0141149819
_diffrn_orient_matrix_UB_32      -0.0294082767
_diffrn_orient_matrix_UB_33      0.0240249096
_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  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            40805
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.91
_exptl_absorpt_coefficient_mu    0.259
_exptl_absorpt_correction_T_max  0.9524
_exptl_absorpt_correction_T_min  0.9356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.31.5 
(release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) 
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         8309
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0328P)^2^+4.2325P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                6615
_reflns_number_total             8309
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8003239-file003_5.cif
_cod_data_source_block           newrm103a
_cod_database_code               4305340