#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:55:19 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179769 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/65/7006544.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_7006544
loop_
_publ_author_name
'Wolf, Robert'
'Finger, Markus'
'Limburg, Carolin'
'Willis, Anthony C.'
'Wild, S. Bruce'
'Hey-Hawkins, Evamarie'
_publ_section_title
;
 Reactivity of cyclooligophosphanes: synthesis and structural
 characterisation of cyclo-1,4-(BH3)2(P4Ph4CH2) and
 cyclo-1,2-(BH3)2(P5Ph5).
;
_journal_issue                   6
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              831
_journal_page_last               837
_journal_paper_doi               10.1039/b511833f
_journal_year                    2006
_chemical_formula_sum            'C30 H31 B2 P5'
_chemical_formula_weight         568.02
_chemical_name_systematic
;
?
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 108.435(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   10.775(5)
_cell_length_b                   22.123(5)
_cell_length_c                   13.275(5)
_cell_measurement_reflns_used    131
_cell_measurement_temperature    207
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      1.84
_cell_volume                     3002.0(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL PLUS'
_computing_publication_material  'WINGX v1.64.05 (Farrugia et al, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      486(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_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  0.0275
_diffrn_reflns_av_sigmaI/netI    0.0365
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19111
_diffrn_reflns_theta_full        29.46
_diffrn_reflns_theta_max         29.46
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.323
_exptl_absorpt_correction_T_max  0.8815
_exptl_absorpt_correction_T_min  0.8815
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.283
_refine_diff_density_min         -0.262
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    located
_refine_ls_matrix_type           full
_refine_ls_number_parameters     458
_refine_ls_number_reflns         7494
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0506P)²+0.5794P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0900
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                5457
_reflns_number_total             7494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b511833f.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7006544
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.53114(17) 0.23287(8) 0.25290(14) 0.0311(4) Uani 1 1 d . . .
C2 C 0.43092(19) 0.25220(8) 0.16375(15) 0.0346(4) Uani 1 1 d . . .
C3 C 0.3311(2) 0.28818(9) 0.17513(17) 0.0414(5) Uani 1 1 d . . .
C4 C 0.3284(2) 0.30359(10) 0.27529(18) 0.0466(5) Uani 1 1 d . . .
C5 C 0.4264(2) 0.28438(11) 0.36344(19) 0.0510(6) Uani 1 1 d . . .
C6 C 0.5286(2) 0.24967(10) 0.35361(17) 0.0423(5) Uani 1 1 d . . .
C7 C 0.41442(17) 0.10068(8) 0.19331(14) 0.0313(4) Uani 1 1 d . . .
C8 C 0.33959(19) 0.12044(9) 0.25568(16) 0.0375(4) Uani 1 1 d . . .
C9 C 0.2090(2) 0.13535(10) 0.20874(19) 0.0460(5) Uani 1 1 d . . .
C10 C 0.1530(2) 0.13077(11) 0.10039(19) 0.0507(5) Uani 1 1 d . . .
C11 C 0.2253(2) 0.11018(11) 0.03831(18) 0.0495(5) Uani 1 1 d . . .
C12 C 0.3557(2) 0.09517(9) 0.08412(16) 0.0384(4) Uani 1 1 d . . .
C13 C 0.79133(19) -0.00814(8) 0.24231(15) 0.0368(4) Uani 1 1 d . . .
C14 C 0.7734(3) -0.07061(10) 0.23648(19) 0.0483(5) Uani 1 1 d . . .
C15 C 0.8700(3) -0.10804(12) 0.3010(2) 0.0632(7) Uani 1 1 d . . .
C16 C 0.9806(3) -0.08449(13) 0.3700(2) 0.0619(7) Uani 1 1 d . . .
C17 C 0.9998(2) -0.02275(13) 0.37646(18) 0.0543(6) Uani 1 1 d . . .
C18 C 0.9055(2) 0.01564(11) 0.31255(17) 0.0453(5) Uani 1 1 d . . .
C19 C 0.74718(19) 0.07899(8) -0.04051(14) 0.0327(4) Uani 1 1 d . . .
C20 C 0.6250(2) 0.08203(9) -0.11753(16) 0.0403(4) Uani 1 1 d . . .
C21 C 0.6079(3) 0.06139(10) -0.21988(17) 0.0487(5) Uani 1 1 d . . .
C22 C 0.7112(3) 0.03776(10) -0.24589(19) 0.0565(7) Uani 1 1 d . . .
C23 C 0.8327(3) 0.03433(11) -0.1707(2) 0.0581(7) Uani 1 1 d . . .
C24 C 0.8511(2) 0.05454(9) -0.06808(18) 0.0440(5) Uani 1 1 d . . .
C25 C 0.74543(17) 0.24592(8) 0.06659(14) 0.0327(4) Uani 1 1 d . . .
C26 C 0.8786(2) 0.25306(11) 0.12222(18) 0.0451(5) Uani 1 1 d . . .
C27 C 0.9410(3) 0.30615(12) 0.1104(2) 0.0581(6) Uani 1 1 d . . .
C28 C 0.8743(3) 0.35198(12) 0.0466(2) 0.0583(7) Uani 1 1 d . . .
C29 C 0.7442(3) 0.34527(11) -0.0083(2) 0.0554(6) Uani 1 1 d . . .
C30 C 0.6793(2) 0.29225(9) 0.00061(17) 0.0430(5) Uani 1 1 d . . .
P1 P 0.66196(4) 0.18365(2) 0.24494(4) 0.02939(11) Uani 1 1 d . . .
P2 P 0.58877(5) 0.09123(2) 0.25963(4) 0.02976(11) Uani 1 1 d . . .
P3 P 0.66098(5) 0.03637(2) 0.14932(4) 0.03170(12) Uani 1 1 d . . .
P4 P 0.78454(5) 0.10388(2) 0.09834(4) 0.03188(12) Uani 1 1 d . . .
P5 P 0.64477(4) 0.18035(2) 0.07497(4) 0.02908(11) Uani 1 1 d . . .
B1 B 0.8297(2) 0.19868(13) 0.3519(2) 0.0446(6) Uani 1 1 d . . .
B2 B 0.6340(3) 0.06557(13) 0.40790(19) 0.0460(6) Uani 1 1 d . . .
H1 H 0.849(2) 0.2472(11) 0.3404(17) 0.054(6) Uiso 1 1 d . . .
H2 H 0.814(2) 0.1882(10) 0.428(2) 0.062(7) Uiso 1 1 d . . .
H2A H 0.431(2) 0.2400(10) 0.0956(18) 0.050(6) Uiso 1 1 d . . .
H3 H 0.902(2) 0.1681(10) 0.3337(18) 0.056(6) Uiso 1 1 d . . .
H3A H 0.267(2) 0.3014(10) 0.1153(19) 0.053(7) Uiso 1 1 d . . .
H4 H 0.604(3) 0.1018(11) 0.447(2) 0.071(8) Uiso 1 1 d . . .
H4A H 0.263(2) 0.3296(11) 0.2837(19) 0.063(7) Uiso 1 1 d . . .
H5 H 0.581(2) 0.0249(11) 0.4105(18) 0.060(7) Uiso 1 1 d . . .
H5A H 0.422(3) 0.2909(12) 0.429(2) 0.073(8) Uiso 1 1 d . . .
H6 H 0.736(3) 0.0622(12) 0.433(2) 0.075(8) Uiso 1 1 d . . .
H6A H 0.593(2) 0.2372(10) 0.4105(19) 0.054(7) Uiso 1 1 d . . .
H8 H 0.378(2) 0.1231(10) 0.3279(18) 0.048(6) Uiso 1 1 d . . .
H9 H 0.163(2) 0.1502(10) 0.2513(19) 0.055(7) Uiso 1 1 d . . .
H10 H 0.068(3) 0.1421(11) 0.071(2) 0.064(7) Uiso 1 1 d . . .
H11 H 0.190(3) 0.1069(12) -0.033(2) 0.071(8) Uiso 1 1 d . . .
H12 H 0.406(2) 0.0810(10) 0.0409(17) 0.049(6) Uiso 1 1 d . . .
H14 H 0.700(2) -0.0861(11) 0.1889(19) 0.054(7) Uiso 1 1 d . . .
H15 H 0.854(3) -0.1484(13) 0.295(2) 0.070(8) Uiso 1 1 d . . .
H16 H 1.053(3) -0.1083(12) 0.416(2) 0.073(8) Uiso 1 1 d . . .
H17 H 1.075(3) -0.0060(12) 0.423(2) 0.065(8) Uiso 1 1 d . . .
H18 H 0.918(2) 0.0568(12) 0.318(2) 0.066(8) Uiso 1 1 d . . .
H20 H 0.550(2) 0.0987(10) -0.1007(17) 0.048(6) Uiso 1 1 d . . .
H21 H 0.523(2) 0.0627(10) -0.2705(19) 0.055(7) Uiso 1 1 d . . .
H22 H 0.695(2) 0.0243(10) -0.3181(19) 0.054(6) Uiso 1 1 d . . .
H23 H 0.900(3) 0.0188(12) -0.185(2) 0.068(8) Uiso 1 1 d . . .
H24 H 0.932(2) 0.0526(9) -0.0150(16) 0.041(6) Uiso 1 1 d . . .
H26 H 0.9213(19) 0.2211(9) 0.1663(16) 0.034(5) Uiso 1 1 d . . .
H27 H 1.023(3) 0.3082(11) 0.147(2) 0.061(8) Uiso 1 1 d . . .
H28 H 0.915(3) 0.3878(12) 0.039(2) 0.073(8) Uiso 1 1 d . . .
H29 H 0.695(2) 0.3759(12) -0.055(2) 0.065(7) Uiso 1 1 d . . .
H30 H 0.591(2) 0.2878(10) -0.0360(18) 0.049(6) Uiso 1 1 d . . .
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'
B B 0.0013 0.0007 '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'
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 C6 119.15(17) . . ?
C2 C1 P1 122.93(14) . . ?
C6 C1 P1 117.85(14) . . ?
C3 C2 C1 120.27(18) . . ?
C4 C3 C2 120.04(19) . . ?
C5 C4 C3 119.9(2) . . ?
C4 C5 C6 120.9(2) . . ?
C5 C6 C1 119.7(2) . . ?
C12 C7 C8 119.19(18) . . ?
C12 C7 P2 123.67(15) . . ?
C8 C7 P2 116.82(14) . . ?
C9 C8 C7 120.1(2) . . ?
C10 C9 C8 120.0(2) . . ?
C9 C10 C11 120.3(2) . . ?
C10 C11 C12 120.3(2) . . ?
C11 C12 C7 120.06(19) . . ?
C18 C13 C14 119.3(2) . . ?
C18 C13 P3 125.07(15) . . ?
C14 C13 P3 115.54(17) . . ?
C15 C14 C13 119.4(3) . . ?
C16 C15 C14 120.9(3) . . ?
C15 C16 C17 120.3(2) . . ?
C16 C17 C18 120.0(3) . . ?
C17 C18 C13 120.0(2) . . ?
C20 C19 C24 118.58(19) . . ?
C20 C19 P4 125.33(15) . . ?
C24 C19 P4 116.09(16) . . ?
C21 C20 C19 120.4(2) . . ?
C22 C21 C20 120.3(2) . . ?
C21 C22 C23 120.1(2) . . ?
C22 C23 C24 120.2(2) . . ?
C23 C24 C19 120.4(2) . . ?
C30 C25 C26 119.03(19) . . ?
C30 C25 P5 115.22(15) . . ?
C26 C25 P5 125.73(15) . . ?
C27 C26 C25 119.3(2) . . ?
C28 C27 C26 121.2(2) . . ?
C29 C28 C27 119.9(2) . . ?
C28 C29 C30 120.3(2) . . ?
C25 C30 C29 120.3(2) . . ?
C1 P1 B1 114.59(10) . . ?
C1 P1 P5 105.34(6) . . ?
B1 P1 P5 120.76(9) . . ?
C1 P1 P2 104.11(6) . . ?
B1 P1 P2 111.56(9) . . ?
P5 P1 P2 98.16(2) . . ?
C7 P2 B2 114.28(10) . . ?
C7 P2 P1 101.12(6) . . ?
B2 P2 P1 111.90(9) . . ?
C7 P2 P3 105.50(6) . . ?
B2 P2 P3 118.46(9) . . ?
P1 P2 P3 103.69(3) . . ?
C13 P3 P2 101.69(7) . . ?
C13 P3 P4 99.16(7) . . ?
P2 P3 P4 101.53(3) . . ?
C19 P4 P5 99.44(6) . . ?
C19 P4 P3 98.06(6) . . ?
P5 P4 P3 96.22(4) . . ?
C25 P5 P1 100.12(6) . . ?
C25 P5 P4 102.88(7) . . ?
P1 P5 P4 92.78(2) . . ?
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 1.393(3) . ?
C1 C6 1.396(3) . ?
C1 P1 1.8104(19) . ?
C2 C3 1.384(3) . ?
C3 C4 1.382(3) . ?
C4 C5 1.373(3) . ?
C5 C6 1.382(3) . ?
C7 C12 1.391(3) . ?
C7 C8 1.396(3) . ?
C7 P2 1.817(2) . ?
C8 C9 1.386(3) . ?
C9 C10 1.376(3) . ?
C10 C11 1.379(3) . ?
C11 C12 1.383(3) . ?
C13 C18 1.391(3) . ?
C13 C14 1.394(3) . ?
C13 P3 1.8355(19) . ?
C14 C15 1.393(3) . ?
C15 C16 1.356(4) . ?
C16 C17 1.380(4) . ?
C17 C18 1.389(3) . ?
C19 C20 1.390(3) . ?
C19 C24 1.392(3) . ?
C19 P4 1.8420(19) . ?
C20 C21 1.389(3) . ?
C21 C22 1.369(4) . ?
C22 C23 1.374(4) . ?
C23 C24 1.387(3) . ?
C25 C30 1.390(3) . ?
C25 C26 1.399(3) . ?
C25 P5 1.8356(19) . ?
C26 C27 1.387(3) . ?
C27 C28 1.370(4) . ?
C28 C29 1.368(4) . ?
C29 C30 1.390(3) . ?
P1 B1 1.941(2) . ?
P1 P5 2.2060(11) . ?
P1 P2 2.2221(8) . ?
P2 B2 1.956(2) . ?
P2 P3 2.2234(8) . ?
P3 P4 2.2430(8) . ?
P4 P5 2.2207(8) . ?
