Synthesis and Coordination Properties of New Bis(phosphinomethyl)pyridine N,P,P'-Trioxides
Xin-Min Gan; Eileen N. Duesler; Robert T. Paine; Inorganic Chemistry 40 (2001) 4420–4427; doi:10.1021/ic0103493

data_4320125
_publ_contact_author             'Robert T. Paine'
_publ_contact_author_email       rtpaine@unm.edu
_publ_contact_author_fax         1.505.277.2609
_publ_contact_author_phone       1.505.277.1661
_publ_section_title
;
 Synthesis and Coordination Properties of New Bis(phosphinomethyl)pyridine
 N,P,P'-Trioxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4420
_journal_page_last               4427
_journal_paper_doi               10.1021/ic0103493
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C72 H78 N6 Nd O17.5 P4'
_chemical_formula_weight         1575.52
_chemical_name_systematic
;
 ?
;
_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
_cell_angle_alpha                68.35(2)
_cell_angle_beta                 68.540(10)
_cell_angle_gamma                81.42(2)
_cell_formula_units_Z            2
_cell_length_a                   15.133(4)
_cell_length_b                   15.930(3)
_cell_length_c                   19.947(5)
_cell_measurement_reflns_used    48
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      2.33
_cell_volume                     4159.0(18)
_computing_cell_refinement       'Siemens XSCANS, 1991'
_computing_data_collection       'Siemens XSCANS, 1991'
_computing_data_reduction        'Siemens XSCANS, 1991'
_computing_molecular_graphics    'Siemens SHELXTL, Version 5, 1994'
_computing_publication_material  'Siemens SHELXTL, Version 5, 1994'
_computing_structure_refinement  'Siemens SHELXTL, Version 5, 1994'
_computing_structure_solution    'Siemens SHELXTL, Version 5, 1994'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_sigmaI/netI    0.1463
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12498
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.52
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.9965
_exptl_absorpt_correction_T_min  0.9091
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_density_method    none
_exptl_crystal_description       rod
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.920
_exptl_crystal_size_mid          0.207
_exptl_crystal_size_min          0.161
_refine_diff_density_max         1.155
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.001
_refine_ls_goodness_of_fit_obs   1.282
_refine_ls_hydrogen_treatment
;
 All hydrogens included in idealized positions [riding model except for
 water hydrogen atoms. These were not found in difference maps.  The
hydrogen
 atom positions for the CH3CN were included [one reasonable position found
 and optimized, other two added in idealized positions] in fixed positions.
 All hydrogen atoms refined with fixed isotropic U's set to
1.25U(equivalent)
 or 1.25U(isotropic) of parent atom.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         10554
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.036
_refine_ls_restrained_S_obs      1.281
_refine_ls_R_factor_all          0.1082
_refine_ls_R_factor_obs          0.0624
_refine_ls_shift/esd_max         -0.095
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1823
_refine_ls_wR_factor_obs         0.1654
_reflns_number_observed          5954
_reflns_number_total             10556
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0103493_2.cif
_cod_data_source_block           rtp983
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4159.0(17)
_cod_database_code               4320125