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_4320785
_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
;
_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            'C42 H48 N3 Nd O14 P2'
_chemical_formula_weight         1025.01
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 103.810(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.417(3)
_cell_length_b                   16.661(2)
_cell_length_c                   15.994(2)
_cell_measurement_reflns_used    49
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.50
_cell_measurement_theta_min      2.27
_cell_volume                     4765.8(12)
_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  0.0457
_diffrn_reflns_av_sigmaI/netI    0.2020
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            9015
_diffrn_reflns_theta_max         24.00
_diffrn_reflns_theta_min         1.79
_diffrn_standards_decay_%        7.5%
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.903
_exptl_absorpt_correction_type   'emprical via \y scans'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2092
_exptl_crystal_size_max          0.276
_exptl_crystal_size_mid          0.253
_exptl_crystal_size_min          0.230
_refine_diff_density_max         0.527
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.065
_refine_ls_goodness_of_fit_obs   1.335
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7475
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.065
_refine_ls_restrained_S_obs      1.334
_refine_ls_R_factor_all          0.1077
_refine_ls_R_factor_obs          0.0403
_refine_ls_shift/esd_max         -0.186
_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc exp(6(sin\q/\l)^2^)/[\s^2^(Fo^2^)+(0.004P)^2^] where P=1/3Fo^2^+2/3Fc^2^'
_refine_ls_wR_factor_all         0.0894
_refine_ls_wR_factor_obs         0.0725
_reflns_number_observed          3397
_reflns_number_total             7475
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0107633_2.cif
_cod_data_source_block           rtp976b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4765.8(11)
_cod_database_code               4320785