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_4320127
_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
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_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            'C33 H31 N4 Nd O12 P2'
_chemical_formula_weight         881.80
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'Patterson map interpretation'
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.766(7)
_cell_length_b                   13.696(3)
_cell_length_c                   10.532(2)
_cell_measurement_reflns_used    68
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.73
_cell_measurement_theta_min      1.65
_cell_volume                     3572.4(14)
_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 scans'
_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  0.0227
_diffrn_reflns_av_sigmaI/netI    0.0513
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8648
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.611
_exptl_absorpt_correction_T_max  0.958
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_density_method    none
_exptl_crystal_description       'irregular chip'
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.460
_exptl_crystal_size_mid          0.391
_exptl_crystal_size_min          0.253
_refine_diff_density_max         0.735
_refine_diff_density_min         -0.562
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.023(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.003
_refine_ls_goodness_of_fit_obs   1.108
_refine_ls_hydrogen_treatment
;
 idealized positions [Riding model] with isotropic U's
 set to 1.25 U(equiv) of parent atom.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         8195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_restrained_S_obs      1.108
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_obs          0.0307
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0638
_refine_ls_wR_factor_obs         0.0625
_reflns_number_observed          6553
_reflns_number_total             8195
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0103493_4.cif
_cod_data_source_block           rtp97c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0200P)^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^)+(0.0200P)^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        3572.1(15)
_cod_database_code               4320127