Synthesis and Coordination Chemistry of 2,6-Bis(diphenylphosphinomethyl)phenol P,P'-Dioxides
Robert T. Paine; Yun-Chou Tan; Xin-Min Gan; Inorganic Chemistry 40 (2001) 7009–7013; doi:10.1021/ic0107633

data_4320784
_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 Chemistry of
 2,6-Bis(diphenylphosphinomethyl)phenol P,P'-Dioxides
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7009
_journal_page_last               7013
_journal_paper_doi               10.1021/ic0107633
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C36 H36 Er N3 O13 P2'
_chemical_formula_weight         947.88
_space_group_IT_number           82
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4'
_symmetry_space_group_name_H-M   'I -4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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            8
_cell_length_a                   28.844(3)
_cell_length_b                   28.844(3)
_cell_length_c                   10.575(1)
_cell_measurement_reflns_used    64
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.98
_cell_measurement_theta_min      2.86
_cell_volume                     8798.1(15)
_computing_cell_refinement       'Siemens XSCANS, 1991'
_computing_data_collection       'Siemens XSCANS, 1991'
_computing_data_reduction        'Siemens XSCANS, 1991'
_computing_molecular_graphics    'Siemens SHELXTL Versions 5, 1994'
_computing_publication_material  'Siemens SHELXTL Versions 5, 1994'
_computing_structure_refinement  'Siemens SHELXTL Versions 5, 1994'
_computing_structure_solution    'Siemens SHELXTL Versions 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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.1421
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11366
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        8.51%
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.040
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.758
_exptl_absorpt_correction_type   'empirical psi-scans'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.035(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.053
_refine_ls_goodness_of_fit_obs   1.390
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         10111
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_restrained_S_obs      1.390
_refine_ls_R_factor_all          0.0930
_refine_ls_R_factor_obs          0.0473
_refine_ls_shift/esd_max         -0.001
_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         0.1073
_refine_ls_wR_factor_obs         0.0983
_reflns_number_observed          5525
_reflns_number_total             10113
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0107633_1.cif
_cod_data_source_block           rtp97a
_cod_depositor_comments
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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 
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_cod_database_code               4320784