#------------------------------------------------------------------------------
#$Date: 2018-09-07 13:54:24 +0300 (Fri, 07 Sep 2018) $
#$Revision: 210528 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/40/7104027.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7104027
loop_
_publ_author_name
'Liddle, Stephen T.'
'Izod, Keith'
_publ_section_title
;
 The first structurally authenticated alkali metal 1,3-diphosphaallyl
 complex [{ButC(PMes)2}Li(thf)3] (Mes = 2,4,6-Me3C6H2): an alternative
 synthetic approach to substituted 1,3-diphosphaallyl complexes
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   6
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              772
_journal_page_last               773
_journal_paper_doi               10.1039/b300272a
_journal_year                    2003
_chemical_formula_moiety         '[MesP=C(But)P(X)Mes]'
_chemical_formula_sum            'C23 H31 Br0.36 Cl0.64 P2'
_chemical_formula_weight         420.87
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.001(2)
_cell_angle_beta                 92.033(2)
_cell_angle_gamma                98.202(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8412(6)
_cell_length_b                   9.4818(6)
_cell_length_c                   14.4128(10)
_cell_measurement_reflns_used    7352
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.29
_cell_volume                     1126.37(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0189
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8092
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.912
_exptl_absorpt_correction_T_max  0.7589
_exptl_absorpt_correction_T_min  0.5290
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             445
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.70
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.317
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       0
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0386P)²+0.5733P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                3422
_reflns_number_total             3930
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b300272a.txt
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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
_cod_database_code               7104027
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6359(2) 0.8381(2) 0.76225(14) 0.0232(4) Uani 1 1 d . A .
C2 C 0.4958(2) 0.7154(2) 0.75591(15) 0.0289(4) Uani 1 1 d . . .
C3 C 0.3606(2) 0.7201(2) 0.68766(17) 0.0369(5) Uani 1 1 d . . .
H3A H 0.2763 0.6390 0.6845 0.055 Uiso 1 1 calc R . .
H3B H 0.3935 0.7063 0.6215 0.055 Uiso 1 1 calc R . .
H3C H 0.3258 0.8181 0.7134 0.055 Uiso 1 1 calc R . .
C4 C 0.5474(3) 0.5593(2) 0.71901(17) 0.0369(5) Uani 1 1 d . . .
H4A H 0.4614 0.4806 0.7173 0.055 Uiso 1 1 calc R . .
H4B H 0.6326 0.5570 0.7636 0.055 Uiso 1 1 calc R . .
H4C H 0.5810 0.5411 0.6526 0.055 Uiso 1 1 calc R . .
C5 C 0.4358(3) 0.7330(3) 0.85729(17) 0.0390(5) Uani 1 1 d . . .
H5A H 0.3457 0.6556 0.8499 0.058 Uiso 1 1 calc R . .
H5B H 0.4072 0.8335 0.8851 0.058 Uiso 1 1 calc R . .
H5C H 0.5162 0.7211 0.9014 0.058 Uiso 1 1 calc R . .
Br1 Br 0.64052(4) 0.68788(4) 0.52158(2) 0.03320(14) Uani 0.363(2) 1 d P A 1
Cl1 Cl 0.64052(4) 0.68788(4) 0.52158(2) 0.03320(14) Uani 0.637(2) 1 d P A 2
P1 P 0.76772(5) 0.81986(5) 0.66489(4) 0.02302(14) Uani 1 1 d . . .
C6 C 0.8065(2) 1.0023(2) 0.64488(13) 0.0218(4) Uani 1 1 d . A .
C7 C 0.9618(2) 1.0511(2) 0.63484(13) 0.0258(4) Uani 1 1 d . . .
C8 C 1.0027(2) 1.1903(2) 0.62254(14) 0.0318(5) Uani 1 1 d . A .
H8A H 1.1077 1.2244 0.6181 0.038 Uiso 1 1 calc R . .
C9 C 0.8958(3) 1.2812(2) 0.61656(16) 0.0349(5) Uani 1 1 d . . .
C10 C 0.7428(2) 1.2273(2) 0.62120(15) 0.0310(5) Uani 1 1 d . A .
H10A H 0.6677 1.2864 0.6142 0.037 Uiso 1 1 calc R . .
C11 C 0.6951(2) 1.0909(2) 0.63559(13) 0.0243(4) Uani 1 1 d . . .
C12 C 1.0875(2) 0.9585(3) 0.63473(16) 0.0357(5) Uani 1 1 d . A .
H12A H 1.1800 1.0031 0.6125 0.054 Uiso 1 1 calc R . .
H12B H 1.0538 0.8547 0.5901 0.054 Uiso 1 1 calc R . .
H12C H 1.1101 0.9574 0.7015 0.054 Uiso 1 1 calc R . .
C13 C 0.9422(3) 1.4314(3) 0.6017(2) 0.0590(8) Uani 1 1 d . A .
H13A H 1.0387 1.4310 0.5702 0.088 Uiso 1 1 calc R . .
H13B H 0.9563 1.5126 0.6656 0.088 Uiso 1 1 calc R . .
H13C H 0.8619 1.4480 0.5596 0.088 Uiso 1 1 calc R . .
C14 C 0.5258(2) 1.0447(2) 0.63945(16) 0.0307(4) Uani 1 1 d . A .
H14A H 0.4694 1.1169 0.6236 0.046 Uiso 1 1 calc R . .
H14B H 0.5061 1.0437 0.7057 0.046 Uiso 1 1 calc R . .
H14C H 0.4917 0.9435 0.5915 0.046 Uiso 1 1 calc R . .
P2 P 0.69699(6) 0.96343(6) 0.87577(4) 0.02930(15) Uani 1 1 d . . .
C15 C 0.8884(2) 1.0654(2) 0.87206(13) 0.0267(4) Uani 1 1 d . A .
C16 C 1.0191(2) 0.9981(2) 0.87672(13) 0.0280(4) Uani 1 1 d . . .
C17 C 1.1635(2) 1.0860(2) 0.88884(14) 0.0312(5) Uani 1 1 d . A .
H17A H 1.2519 1.0408 0.8921 0.037 Uiso 1 1 calc R . .
C18 C 1.1831(2) 1.2371(2) 0.89625(14) 0.0336(5) Uani 1 1 d . . .
C19 C 1.0526(2) 1.3032(2) 0.89555(14) 0.0328(5) Uani 1 1 d . A .
H19A H 1.0640 1.4074 0.9024 0.039 Uiso 1 1 calc R . .
C20 C 0.9064(2) 1.2211(2) 0.88504(14) 0.0293(4) Uani 1 1 d . . .
C21 C 1.0088(2) 0.8341(2) 0.86890(15) 0.0321(5) Uani 1 1 d . A .
H21A H 1.1085 0.8166 0.8909 0.048 Uiso 1 1 calc R . .
H21B H 0.9803 0.7696 0.8003 0.048 Uiso 1 1 calc R . .
H21C H 0.9310 0.8096 0.9105 0.048 Uiso 1 1 calc R . .
C22 C 1.3413(3) 1.3267(3) 0.9044(2) 0.0503(6) Uani 1 1 d . A .
H22A H 1.3509 1.4218 0.9597 0.076 Uiso 1 1 calc R . .
H22B H 1.3576 1.3486 0.8433 0.076 Uiso 1 1 calc R . .
H22C H 1.4184 1.2679 0.9157 0.076 Uiso 1 1 calc R . .
C23 C 0.7686(3) 1.3006(2) 0.88918(16) 0.0378(5) Uani 1 1 d . A .
H23A H 0.8028 1.4059 0.8939 0.057 Uiso 1 1 calc R . .
H23B H 0.7145 1.2980 0.9469 0.057 Uiso 1 1 calc R . .
H23C H 0.6993 1.2493 0.8293 0.057 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C2 C1 P1 122.85(13) . . ?
C2 C1 P2 116.49(14) . . ?
P1 C1 P2 118.05(10) . . ?
C1 C2 C3 112.44(16) . . ?
C1 C2 C4 108.32(16) . . ?
C1 C2 C5 111.95(17) . . ?
C3 C2 C4 110.17(18) . . ?
C3 C2 C5 106.93(17) . . ?
C4 C2 C5 106.89(16) . . ?
C1 P1 Br1 109.15(6) . . ?
C1 P1 C6 107.82(8) . . ?
Br1 P1 C6 97.94(6) . . ?
P1 C6 C7 114.98(14) . . ?
P1 C6 C11 125.49(14) . . ?
C7 C6 C11 119.49(17) . . ?
C6 C7 C8 118.97(18) . . ?
C6 C7 C12 123.60(18) . . ?
C8 C7 C12 117.42(18) . . ?
C7 C8 C9 122.31(18) . . ?
C8 C9 C10 117.74(19) . . ?
C8 C9 C13 121.5(2) . . ?
C10 C9 C13 120.7(2) . . ?
C9 C10 C11 122.66(19) . . ?
C6 C11 C10 118.67(17) . . ?
C6 C11 C14 123.59(17) . . ?
C10 C11 C14 117.74(17) . . ?
C1 P2 C15 109.18(9) . . ?
P2 C15 C16 120.05(15) . . ?
P2 C15 C20 119.17(14) . . ?
C16 C15 C20 119.49(18) . . ?
C15 C16 C17 118.69(19) . . ?
C15 C16 C21 122.55(18) . . ?
C17 C16 C21 118.76(18) . . ?
C16 C17 C18 122.44(19) . . ?
C17 C18 C19 118.00(19) . . ?
C17 C18 C22 120.9(2) . . ?
C19 C18 C22 121.1(2) . . ?
C18 C19 C20 121.7(2) . . ?
C15 C20 C19 119.47(18) . . ?
C15 C20 C23 121.09(19) . . ?
C19 C20 C23 119.43(19) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.552(3) . ?
C1 P1 1.8362(19) . ?
C1 P2 1.6938(19) . ?
C2 C3 1.536(3) . ?
C2 C4 1.542(3) . ?
C2 C5 1.538(3) . ?
Br1 P1 2.2018(6) . ?
P1 C6 1.8321(19) . ?
C6 C7 1.413(3) . ?
C6 C11 1.412(3) . ?
C7 C8 1.387(3) . ?
C7 C12 1.511(3) . ?
C8 C9 1.385(3) . ?
C9 C10 1.388(3) . ?
C9 C13 1.510(3) . ?
C10 C11 1.385(3) . ?
C11 C14 1.507(3) . ?
P2 C15 1.837(2) . ?
C15 C16 1.407(3) . ?
C15 C20 1.411(3) . ?
C16 C17 1.394(3) . ?
C16 C21 1.512(3) . ?
C17 C18 1.386(3) . ?
C18 C19 1.390(3) . ?
C18 C22 1.509(3) . ?
C19 C20 1.387(3) . ?
C20 C23 1.514(3) . ?
