Vicinal diphosphoniums: electrostatic repulsion under covalent constraint
Abdalilah, Mohammed; Zurawinski, Remigiuz; Canac, Yves; Laleu, Benoît; Lacour, Jérôme; Lepetit, Christine; Magro, Germinal; Bernardinelli, Gérald; Donnadieu, Bruno; Duhayon, Carine; Mikolajczyk, Marian; Chauvin, Remi; Dalton Transactions  (2009) 8493–8508; doi:10.1039/b903933c

data_7002427
_publ_section_title
;
 Vicinal diphosphoniums: electrostatic repulsion under covalent
 constraint
;
_journal_issue                   40
_journal_name_full               'Dalton Transactions'
_journal_page_first              8493
_journal_page_last               8508
_journal_paper_doi               10.1039/b903933c
_journal_year                    2009
_chemical_compound_source
;
?
;
_chemical_formula_moiety         ' C33 H30 P2, C3 H6 O, 2(I) '
_chemical_formula_sum            'C36 H36 I2 O P2'
_chemical_formula_weight         800.39
_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
_audit_creation_date             04-25-05
_audit_creation_method           CRYSTALS_ver_12-03-99
_cell_angle_alpha                90
_cell_angle_beta                 101.602(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.1216(9)
_cell_length_b                   16.4811(14)
_cell_length_c                   26.8178(15)
_cell_measurement_reflns_used    7995
_cell_measurement_temperature    180
_cell_measurement_theta_max      26.06
_cell_measurement_theta_min      2.05
_cell_volume                     6979.9(8)
_computing_cell_refinement
;
IPDS (Stoe & Cie, 1996)
;
_computing_data_collection
;
IPDS (Stoe & Cie, 1996)
;
_computing_data_reduction
;
XRED (Stoe & Cie 1996)
;
_computing_molecular_graphics
;
CAMERON (Watkin et al 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al 2003)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al 2003)
;
_computing_structure_solution
;
SIR92 (Altomare et al, 1994)
;
_diffrn_ambient_temperature      180
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type
;
Stoe IPDS
;
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.03
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            69932
_diffrn_reflns_theta_full        26.059
_diffrn_reflns_theta_max         26.059
_diffrn_reflns_theta_min         2.048
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.920
_exptl_absorpt_correction_T_max  0.75
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            ' colorless '
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_description       ' block '
_exptl_crystal_F_000             3168
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.25
_refine_diff_density_min         -0.56
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1382
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     700
_refine_ls_number_reflns         7431
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0249
_refine_ls_shift/su_max          0.001789
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.08 -0.167 0.707
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0327
_refine_ls_wR_factor_gt          0.0289
_refine_ls_wR_factor_ref         0.0289
_reflns_limit_h_max              19
_reflns_limit_h_min              -19
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              33
_reflns_limit_l_min              0
_reflns_number_gt                7431
_reflns_number_total             13133
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b903933c.txt
_cod_data_source_block           compound5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        ' C36 H36 I2 O1 P2 '
_cod_database_code               7002427