#------------------------------------------------------------------------------
#$Date: 2019-11-28 21:01:50 +0200 (Thu, 28 Nov 2019) $
#$Revision: 244609 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/92/7239232.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_7239232
loop_
_publ_author_name
'Ghalib, Mohammed'
'Jones, Peter G.'
'Palm, Gottfried J.'
'Heinicke, Joachim W.'
_publ_section_title
;
 Phosphanyl-substituted π-excess σ2P heterocycles: Coordination
 behaviour of 2-di-tert-butylphosphanyl-1-neopentyl-1,3-benzazaphosphole
 towards CuCl, HgCl2 and [Rh(COD)2]BF4
;
_journal_issue                   39
_journal_name_full               'RSC Advances'
_journal_page_first              17726
_journal_paper_doi               10.1039/c3ra43706j
_journal_volume                  3
_journal_year                    2013
_chemical_formula_sum            'C28 H46 B F3 N O P2 Rh'
_chemical_formula_weight         645.32
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_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                90.00
_cell_angle_beta                 91.102(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.70896(15)
_cell_length_b                   18.3370(3)
_cell_length_c                   14.9610(2)
_cell_measurement_reflns_used    37610
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.2234
_cell_measurement_theta_min      2.1982
_cell_volume                     2937.35(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            95434
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         7619
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0313
_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)+(0.0355P)²+2.8771P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                6686
_reflns_number_total             7619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra43706j.txt
_cod_data_source_block           grobuu
_cod_depositor_comments
;
The following automatic conversions were performed:

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

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2937.36(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7239232
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
Rh Rh 0.378977(14) 0.170465(8) 0.357379(10) 0.02202(5) Uani 1 1 d .
P1 P 0.44381(5) 0.27541(3) 0.43505(3) 0.02280(10) Uani 1 1 d .
N1 N 0.61800(16) 0.35432(9) 0.31593(11) 0.0246(3) Uani 1 1 d .
C2 C 0.59103(17) 0.28895(10) 0.36498(12) 0.0213(4) Uani 1 1 d .
H2 H 0.6667 0.2731 0.4000 0.026 Uiso 1 1 calc R
P3 P 0.54329(4) 0.21676(3) 0.28572(3) 0.01994(10) Uani 1 1 d .
C3A C 0.51656(17) 0.28587(11) 0.20227(12) 0.0228(4) Uani 1 1 d .
C4 C 0.45727(19) 0.27859(13) 0.11907(13) 0.0303(4) Uani 1 1 d .
H4 H 0.4227 0.2330 0.1014 0.036 Uiso 1 1 calc R
C5 C 0.4489(2) 0.33800(15) 0.06228(15) 0.0371(5) Uani 1 1 d .
H5 H 0.4072 0.3339 0.0059 0.045 Uiso 1 1 calc R
C6 C 0.5022(2) 0.40376(14) 0.08874(15) 0.0358(5) Uani 1 1 d .
H6 H 0.4975 0.4441 0.0490 0.043 Uiso 1 1 calc R
C7 C 0.5620(2) 0.41280(12) 0.17093(14) 0.0304(4) Uani 1 1 d .
H7 H 0.5981 0.4583 0.1872 0.037 Uiso 1 1 calc R
C7A C 0.56786(17) 0.35312(11) 0.22946(13) 0.0233(4) Uani 1 1 d .
C8 C 0.69154(19) 0.41434(11) 0.35410(14) 0.0272(4) Uani 1 1 d .
H8A H 0.6759 0.4164 0.4191 0.033 Uiso 1 1 calc R
H8B H 0.6602 0.4605 0.3277 0.033 Uiso 1 1 calc R
C9 C 0.8347(2) 0.41115(12) 0.34111(17) 0.0353(5) Uani 1 1 d .
C10 C 0.8644(2) 0.41418(16) 0.24188(19) 0.0489(7) Uani 1 1 d .
H10A H 0.9551 0.4122 0.2346 0.073 Uiso 1 1 calc R
H10B H 0.8319 0.4597 0.2162 0.073 Uiso 1 1 calc R
H10C H 0.8254 0.3726 0.2111 0.073 Uiso 1 1 calc R
C11 C 0.8890(2) 0.47877(14) 0.38814(18) 0.0426(6) Uani 1 1 d .
H11A H 0.8722 0.4761 0.4522 0.064 Uiso 1 1 calc R
H11B H 0.8501 0.5227 0.3629 0.064 Uiso 1 1 calc R
H11C H 0.9794 0.4806 0.3794 0.064 Uiso 1 1 calc R
C12 C 0.8905(3) 0.34229(16) 0.3811(3) 0.0619(9) Uani 1 1 d .
H12A H 0.8542 0.2996 0.3508 0.093 Uiso 1 1 calc R
H12B H 0.8721 0.3401 0.4449 0.093 Uiso 1 1 calc R
H12C H 0.9811 0.3425 0.3733 0.093 Uiso 1 1 calc R
C13 C 0.5168(2) 0.26126(12) 0.55027(13) 0.0334(5) Uani 1 1 d .
C14 C 0.5839(3) 0.18770(14) 0.54699(15) 0.0402(5) Uani 1 1 d .
H14A H 0.6238 0.1777 0.6052 0.060 Uiso 1 1 calc R
H14B H 0.6476 0.1891 0.5009 0.060 Uiso 1 1 calc R
H14C H 0.5233 0.1492 0.5328 0.060 Uiso 1 1 calc R
C15 C 0.4181(3) 0.25854(16) 0.62280(16) 0.0483(6) Uani 1 1 d .
H15A H 0.3474 0.2287 0.6020 0.072 Uiso 1 1 calc R
H15B H 0.3891 0.3081 0.6355 0.072 Uiso 1 1 calc R
H15C H 0.4546 0.2371 0.6773 0.072 Uiso 1 1 calc R
C16 C 0.6135(3) 0.31988(16) 0.57560(17) 0.0505(7) Uani 1 1 d .
H16A H 0.5725 0.3676 0.5778 0.076 Uiso 1 1 calc R
H16B H 0.6791 0.3209 0.5308 0.076 Uiso 1 1 calc R
H16C H 0.6506 0.3086 0.6343 0.076 Uiso 1 1 calc R
C17 C 0.3357(2) 0.35672(12) 0.42849(17) 0.0348(5) Uani 1 1 d .
C18 C 0.2800(3) 0.35746(16) 0.33374(18) 0.0493(7) Uani 1 1 d .
H18A H 0.2170 0.3961 0.3287 0.074 Uiso 1 1 calc R
H18B H 0.2410 0.3102 0.3208 0.074 Uiso 1 1 calc R
H18C H 0.3463 0.3666 0.2909 0.074 Uiso 1 1 calc R
C19 C 0.2278(2) 0.34659(15) 0.49358(19) 0.0441(6) Uani 1 1 d .
H19A H 0.2587 0.3539 0.5550 0.066 Uiso 1 1 calc R
H19B H 0.1939 0.2972 0.4874 0.066 Uiso 1 1 calc R
H19C H 0.1620 0.3822 0.4799 0.066 Uiso 1 1 calc R
C20 C 0.3981(3) 0.43006(15) 0.4488(3) 0.0681(10) Uani 1 1 d .
H20A H 0.3361 0.4692 0.4429 0.102 Uiso 1 1 calc R
H20B H 0.4655 0.4384 0.4066 0.102 Uiso 1 1 calc R
H20C H 0.4327 0.4296 0.5099 0.102 Uiso 1 1 calc R
C21 C 0.2653(2) 0.11044(15) 0.46091(15) 0.0411(6) Uani 1 1 d D
H21 H 0.291(3) 0.1333(15) 0.5126(15) 0.049(8) Uiso 1 1 d D
C22 C 0.1858(2) 0.14857(14) 0.40807(18) 0.0399(6) Uani 1 1 d D
H22 H 0.163(3) 0.1942(12) 0.428(2) 0.055(9) Uiso 1 1 d D
C23 C 0.1091(2) 0.11904(15) 0.33208(18) 0.0445(6) Uani 1 1 d .
H23A H 0.0789 0.1604 0.2950 0.053 Uiso 1 1 calc R
H23B H 0.0350 0.0943 0.3565 0.053 Uiso 1 1 calc R
C24 C 0.1764(2) 0.06618(14) 0.27293(16) 0.0394(5) Uani 1 1 d .
H24A H 0.1330 0.0644 0.2140 0.047 Uiso 1 1 calc R
H24B H 0.1720 0.0169 0.2997 0.047 Uiso 1 1 calc R
C25 C 0.3129(2) 0.08572(12) 0.25918(15) 0.0334(5) Uani 1 1 d D
H25 H 0.336(2) 0.1046(14) 0.2058(14) 0.039(7) Uiso 1 1 d D
C26 C 0.4086(2) 0.05867(12) 0.31061(17) 0.0351(5) Uani 1 1 d D
H26 H 0.4863(19) 0.0586(16) 0.2894(18) 0.044(8) Uiso 1 1 d D
C27 C 0.3949(3) 0.00951(15) 0.3901(2) 0.0486(7) Uani 1 1 d .
H27A H 0.4749 0.0093 0.4244 0.058 Uiso 1 1 calc R
H27B H 0.3800 -0.0408 0.3683 0.058 Uiso 1 1 calc R
C28 C 0.2902(2) 0.02995(16) 0.45356(18) 0.0475(7) Uani 1 1 d .
H28A H 0.2124 0.0055 0.4330 0.057 Uiso 1 1 calc R
H28B H 0.3116 0.0109 0.5138 0.057 Uiso 1 1 calc R
B B 0.7506(2) 0.12794(14) 0.30029(16) 0.0300(5) Uani 1 1 d .
O1 O 0.65461(13) 0.17012(7) 0.24904(9) 0.0252(3) Uani 1 1 d .
F2 F 0.82026(13) 0.08945(8) 0.23941(9) 0.0411(3) Uani 1 1 d .
F3 F 0.82621(16) 0.17539(9) 0.34777(12) 0.0550(4) Uani 1 1 d .
F4 F 0.69537(16) 0.08079(11) 0.35933(12) 0.0649(5) Uani 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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
C26 Rh C25 35.77(9)
C26 Rh P3 94.70(6)
C25 Rh P3 100.93(6)
C26 Rh C22 94.59(9)
C25 Rh C22 79.45(9)
P3 Rh C22 164.03(7)
C26 Rh C21 81.20(9)
C25 Rh C21 86.82(9)
P3 Rh C21 160.68(7)
C22 Rh C21 34.61(10)
C26 Rh P1 151.93(7)
C25 Rh P1 168.24(6)
P3 Rh P1 72.490(17)
C22 Rh P1 104.14(7)
C21 Rh P1 102.53(7)
C17 P1 C13 113.37(11)
C17 P1 C2 112.17(9)
C13 P1 C2 100.66(9)
C17 P1 Rh 116.50(8)
C13 P1 Rh 116.79(7)
C2 P1 Rh 94.22(6)
C7A N1 C2 112.56(16)
C7A N1 C8 124.75(16)
C2 N1 C8 122.68(16)
N1 C2 P3 109.05(12)
N1 C2 P1 124.05(14)
P3 C2 P1 92.17(8)
O1 P3 C3A 104.62(8)
O1 P3 C2 114.33(8)
C3A P3 C2 88.80(9)
O1 P3 Rh 124.52(6)
C3A P3 Rh 118.84(6)
C2 P3 Rh 100.05(6)
C4 C3A C7A 120.74(18)
C4 C3A P3 128.08(17)
C7A C3A P3 111.15(14)
C5 C4 C3A 119.8(2)
C4 C5 C6 119.2(2)
C7 C6 C5 122.5(2)
C6 C7 C7A 118.4(2)
N1 C7A C7 125.47(19)
N1 C7A C3A 115.11(17)
C7 C7A C3A 119.39(18)
N1 C8 C9 116.67(17)
C12 C9 C10 109.0(2)
C12 C9 C11 110.4(2)
C10 C9 C11 109.4(2)
C12 C9 C8 111.44(19)
C10 C9 C8 110.3(2)
C11 C9 C8 106.22(19)
C14 C13 C15 109.0(2)
C14 C13 C16 108.1(2)
C15 C13 C16 108.6(2)
C14 C13 P1 106.09(14)
C15 C13 P1 111.76(18)
C16 C13 P1 113.13(16)
C18 C17 C20 109.8(3)
C18 C17 C19 107.7(2)
C20 C17 C19 108.1(2)
C18 C17 P1 106.45(16)
C20 C17 P1 114.73(18)
C19 C17 P1 109.84(17)
C22 C21 C28 125.3(2)
C22 C21 Rh 71.89(13)
C28 C21 Rh 109.13(16)
C21 C22 C23 126.3(2)
C21 C22 Rh 73.49(13)
C23 C22 Rh 107.71(16)
C22 C23 C24 114.7(2)
C23 C24 C25 113.6(2)
C26 C25 C24 123.4(2)
C26 C25 Rh 70.01(13)
C24 C25 Rh 111.47(15)
C25 C26 C27 125.6(2)
C25 C26 Rh 74.22(13)
C27 C26 Rh 106.97(18)
C26 C27 C28 115.3(2)
C21 C28 C27 114.7(2)
F3 B F4 108.7(2)
F3 B F2 110.11(19)
F4 B F2 110.2(2)
F3 B O1 109.33(19)
F4 B O1 110.82(18)
F2 B O1 107.59(18)
B O1 P3 128.56(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Rh C26 2.191(2)
Rh C25 2.244(2)
Rh P3 2.2448(5)
Rh C22 2.253(2)
Rh C21 2.272(2)
Rh P1 2.3462(5)
P1 C17 1.889(2)
P1 C13 1.897(2)
P1 C2 1.9260(19)
N1 C7A 1.391(2)
N1 C2 1.438(2)
N1 C8 1.463(2)
C2 P3 1.8429(19)
P3 O1 1.5745(14)
P3 C3A 1.7980(19)
C3A C4 1.393(3)
C3A C7A 1.407(3)
C4 C5 1.383(3)
C5 C6 1.388(4)
C6 C7 1.385(3)
C7 C7A 1.402(3)
C8 C9 1.550(3)
C9 C12 1.515(4)
C9 C10 1.525(4)
C9 C11 1.535(3)
C13 C14 1.529(4)
C13 C15 1.530(3)
C13 C16 1.535(3)
C17 C18 1.527(4)
C17 C20 1.530(4)
C17 C19 1.536(3)
C21 C22 1.346(4)
C21 C28 1.504(4)
C22 C23 1.492(4)
C23 C24 1.506(4)
C24 C25 1.523(3)
C25 C26 1.363(3)
C26 C27 1.502(3)
C27 C28 1.530(4)
B F3 1.377(3)
B F4 1.378(3)
B F2 1.382(3)
B O1 1.488(3)
