#------------------------------------------------------------------------------
#$Date: 2018-01-24 01:46:27 +0200 (Wed, 24 Jan 2018) $
#$Revision: 205502 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/70/4127066.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_4127066
loop_
_publ_author_name
'Adams, Gemma M.'
'Colebatch, Annie L.'
'Skornia, Joseph T.'
'McKay, Alasdair I.'
'Johnson, Heather C.'
'Lloyd Jones, Guy C.'
'Macgregor, Stuart A.'
'Beattie, Nicholas A.'
'Weller, Andrew S.'
_publ_section_title
;
 Dehydropolymerization of H3B·NMeH2 To Form Polyaminoboranes Using
 [Rh(Xantphos-alkyl)] Catalysts.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b11975
_journal_year                    2018
_chemical_compound_source        SYN
_chemical_formula_moiety         'C46 H64 Cl2 O2 P4 Rh2'
_chemical_formula_sum            'C46 H64 Cl2 O2 P4 Rh2'
_chemical_formula_weight         1049.62
_chemical_melting_point          ?
_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   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-11
_audit_creation_method           CRYSTALS_ver_14.43
_cell_angle_alpha                107.4934(15)
_cell_angle_beta                 98.9909(14)
_cell_angle_gamma                100.2269(13)
_cell_formula_units_Z            1
_cell_length_a                   10.0314(3)
_cell_length_b                   10.5096(3)
_cell_length_c                   12.0652(4)
_cell_measurement_reflns_used    4889
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1163.72(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8854
_diffrn_reflns_theta_full        25.609
_diffrn_reflns_theta_max         27.536
_diffrn_reflns_theta_min         5.125
_diffrn_standards_decay_%        -
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.998
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.89
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            'red-yellow dichromic'
_exptl_crystal_density_diffrn    1.498
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.86
_refine_diff_density_min         -0.95
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9243
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         5309
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.0005241
_refine_ls_shift/su_mean         0.0000175
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 12.4 17.3 8.18 2.11 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0850
_refine_ls_wR_factor_gt          0.0748
_refine_ls_wR_factor_ref         0.0850
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4548
_reflns_number_total             5310
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   1.61
_oxford_diffrn_Wilson_scale      8.27
_oxford_refine_ls_r_factor_ref   0.0430
_oxford_refine_ls_scale          0.3472(3)
_oxford_reflns_number_all        5310
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title 'ALC97 At 11:56 on 11/ 5'
_cod_data_source_file            ja7b11975_si_002.cif
_cod_data_source_block           complex_8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

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

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_sg_symbol_H-M      'P -1 '
_cod_database_code               4127066
_iucr_refine_instructions_details_constraints
;
#
# Punched on 11/05/16 at 12:12:23
#
#LIST     12                                                                    
BLOCK 
CONT SCALE 
CONT C    (    1 ,X'S,U'S)  UNTIL RH   (    1 ) 
CONT H    (   21 ,X'S)  UNTIL H    (  231 ) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
#
# Punched on 11/05/16 at 12:12:23
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
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_occupancy
_atom_site_adp_type
C1 C 0.2268(3) 0.6892(3) 0.3113(3) 0.0200 1.0000 Uani
C2 C 0.3551(3) 0.6943(3) 0.3813(3) 0.0238 1.0000 Uani
C3 C 0.3712(4) 0.5872(4) 0.4236(3) 0.0285 1.0000 Uani
C4 C 0.2597(4) 0.4761(3) 0.4019(3) 0.0268 1.0000 Uani
C5 C 0.1312(3) 0.4656(3) 0.3319(3) 0.0218 1.0000 Uani
C6 C 0.1221(3) 0.5700(3) 0.2850(3) 0.0200 1.0000 Uani
C7 C 0.0025(3) 0.3480(3) 0.3045(3) 0.0224 1.0000 Uani
C8 C 0.0033(4) 0.2895(4) 0.4063(3) 0.0283 1.0000 Uani
C9 C 0.0026(4) 0.2353(3) 0.1880(3) 0.0276 1.0000 Uani
C10 C -0.1267(3) 0.4048(3) 0.2837(3) 0.0224 1.0000 Uani
C11 C -0.2553(4) 0.3541(4) 0.3047(3) 0.0284 1.0000 Uani
C12 C -0.3666(4) 0.4130(4) 0.2848(3) 0.0296 1.0000 Uani
C13 C -0.3514(3) 0.5280(3) 0.2494(3) 0.0243 1.0000 Uani
C14 C -0.2243(3) 0.5828(3) 0.2280(3) 0.0206 1.0000 Uani
C15 C -0.1194(3) 0.5132(3) 0.2402(3) 0.0197 1.0000 Uani
C16 C 0.3418(3) 0.9636(3) 0.3293(3) 0.0227 1.0000 Uani
C17 C 0.3351(4) 1.0929(4) 0.2986(4) 0.0337 1.0000 Uani
C18 C 0.1683(3) 0.7781(4) 0.1091(3) 0.0239 1.0000 Uani
C19 C 0.3015(4) 0.7591(5) 0.0679(3) 0.0336 1.0000 Uani
C20 C -0.3357(3) 0.8078(3) 0.2020(3) 0.0238 1.0000 Uani
C21 C -0.3178(4) 0.9428(4) 0.1764(4) 0.0317 1.0000 Uani
C22 C -0.1761(3) 0.6899(4) 0.0423(3) 0.0243 1.0000 Uani
C23 C -0.3176(4) 0.6173(4) -0.0432(3) 0.0329 1.0000 Uani
Cl1 Cl 0.16298(7) 1.04041(8) 0.53045(7) 0.0251 1.0000 Uani
O1 O 0.0015(2) 0.5628(2) 0.20805(19) 0.0199 1.0000 Uani
P1 P 0.17679(8) 0.83127(8) 0.27016(7) 0.0176 1.0000 Uani
P2 P -0.17442(8) 0.74688(8) 0.20321(7) 0.0183 1.0000 Uani
Rh1 Rh 0.00150(2) 0.88878(2) 0.34931(2) 0.0174 1.0000 Uani
H21 H 0.432(4) 0.779(4) 0.408(4) 0.0282 1.0000 Uiso
H31 H 0.464(4) 0.594(4) 0.473(4) 0.0333 1.0000 Uiso
H41 H 0.273(4) 0.409(4) 0.441(4) 0.0331 1.0000 Uiso
H81 H -0.080(5) 0.208(5) 0.385(4) 0.0427 1.0000 Uiso
H83 H 0.007(5) 0.361(5) 0.483(4) 0.0427 1.0000 Uiso
H82 H 0.087(5) 0.249(5) 0.413(4) 0.0432 1.0000 Uiso
H92 H -0.078(5) 0.163(5) 0.166(4) 0.0418 1.0000 Uiso
H91 H 0.001(5) 0.274(5) 0.122(4) 0.0418 1.0000 Uiso
H93 H 0.086(5) 0.194(5) 0.199(4) 0.0421 1.0000 Uiso
H111 H -0.268(4) 0.277(4) 0.334(4) 0.0344 1.0000 Uiso
H121 H -0.452(5) 0.379(4) 0.302(4) 0.0351 1.0000 Uiso
H131 H -0.432(4) 0.569(4) 0.236(4) 0.0293 1.0000 Uiso
H162 H 0.359(4) 0.981(4) 0.415(4) 0.0266 1.0000 Uiso
H161 H 0.415(4) 0.921(4) 0.299(4) 0.0269 1.0000 Uiso
H172 H 0.427(5) 1.165(5) 0.332(4) 0.0500 1.0000 Uiso
H171 H 0.258(5) 1.129(5) 0.331(4) 0.0503 1.0000 Uiso
H173 H 0.315(5) 1.075(5) 0.212(5) 0.0501 1.0000 Uiso
H181 H 0.132(4) 0.847(4) 0.082(4) 0.0291 1.0000 Uiso
H182 H 0.104(4) 0.695(4) 0.076(4) 0.0290 1.0000 Uiso
H191 H 0.283(5) 0.721(5) -0.021(5) 0.0499 1.0000 Uiso
H193 H 0.367(5) 0.849(5) 0.095(4) 0.0498 1.0000 Uiso
H192 H 0.351(5) 0.701(5) 0.104(4) 0.0500 1.0000 Uiso
H202 H -0.348(4) 0.819(4) 0.282(4) 0.0276 1.0000 Uiso
H201 H -0.413(4) 0.731(4) 0.141(4) 0.0282 1.0000 Uiso
H213 H -0.405(5) 0.979(5) 0.183(4) 0.0482 1.0000 Uiso
H211 H -0.236(5) 1.012(5) 0.237(4) 0.0480 1.0000 Uiso
H212 H -0.303(5) 0.933(5) 0.097(5) 0.0481 1.0000 Uiso
H221 H -0.133(4) 0.776(4) 0.027(4) 0.0300 1.0000 Uiso
H222 H -0.115(4) 0.631(4) 0.031(4) 0.0299 1.0000 Uiso
H232 H -0.308(5) 0.574(5) -0.126(5) 0.0491 1.0000 Uiso
H233 H -0.382(5) 0.686(5) -0.046(4) 0.0487 1.0000 Uiso
H231 H -0.366(5) 0.543(5) -0.015(4) 0.0489 1.0000 Uiso
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Rh -1.1178 0.9187 19.2957 0.7515 14.3501 8.2176 4.7343 25.8749 1.2892 98.6062
5.3280 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 C6 116.1(3) yes
C2 . C1 P1 126.2(2) yes
C6 . C1 P1 117.1(2) yes
C1 . C2 C3 120.3(3) yes
C1 . C2 H21 120(2) no
C3 . C2 H21 119(2) no
C2 . C3 C4 120.8(3) yes
C2 . C3 H31 118(2) no
C4 . C3 H31 121(2) no
C3 . C4 C5 120.9(3) yes
C3 . C4 H41 118(2) no
C5 . C4 H41 121(2) no
C4 . C5 C6 116.3(3) yes
C4 . C5 C7 124.4(3) yes
C6 . C5 C7 119.2(3) yes
C1 . C6 C5 125.2(3) yes
C1 . C6 O1 114.7(3) yes
C5 . C6 O1 120.1(3) yes
C5 . C7 C8 111.2(3) yes
C5 . C7 C9 108.0(3) yes
C8 . C7 C9 110.3(3) yes
C5 . C7 C10 107.7(2) yes
C8 . C7 C10 111.1(3) yes
C9 . C7 C10 108.4(3) yes
C7 . C8 H81 110(3) no
C7 . C8 H83 111(3) no
H81 . C8 H83 112(4) no
C7 . C8 H82 108(3) no
H81 . C8 H82 105(4) no
H83 . C8 H82 111(4) no
C7 . C9 H92 110(3) no
C7 . C9 H91 110(3) no
H92 . C9 H91 107(4) no
C7 . C9 H93 110(3) no
H92 . C9 H93 108(4) no
H91 . C9 H93 112(4) no
C7 . C10 C11 124.6(3) yes
C7 . C10 C15 119.4(3) yes
C11 . C10 C15 115.9(3) yes
C10 . C11 C12 120.8(3) yes
C10 . C11 H111 120(3) no
C12 . C11 H111 119(3) no
C11 . C12 C13 121.1(3) yes
C11 . C12 H121 120(3) no
C13 . C12 H121 119(3) no
C12 . C13 C14 119.9(3) yes
C12 . C13 H131 120(2) no
C14 . C13 H131 120(2) no
C13 . C14 C15 116.5(3) yes
C13 . C14 P2 126.7(2) yes
C15 . C14 P2 116.4(2) yes
C14 . C15 C10 125.2(3) yes
C14 . C15 O1 115.1(3) yes
C10 . C15 O1 119.6(3) yes
C17 . C16 P1 113.1(2) yes
C17 . C16 H162 112(2) no
P1 . C16 H162 104(2) no
C17 . C16 H161 112(2) no
P1 . C16 H161 107(2) no
H162 . C16 H161 108(3) no
C16 . C17 H172 112(3) no
C16 . C17 H171 108(3) no
H172 . C17 H171 111(4) no
C16 . C17 H173 112(3) no
H172 . C17 H173 106(4) no
H171 . C17 H173 108(4) no
C19 . C18 P1 117.6(2) yes
C19 . C18 H181 111(2) no
P1 . C18 H181 106(2) no
C19 . C18 H182 108(3) no
P1 . C18 H182 106(3) no
H181 . C18 H182 109(3) no
C18 . C19 H191 111(3) no
C18 . C19 H193 109(3) no
H191 . C19 H193 108(4) no
C18 . C19 H192 114(3) no
H191 . C19 H192 111(4) no
H193 . C19 H192 105(4) no
C21 . C20 P2 110.8(2) yes
C21 . C20 H202 112(2) no
P2 . C20 H202 102(2) no
C21 . C20 H201 113(2) no
P2 . C20 H201 107(2) no
H202 . C20 H201 111(3) no
C20 . C21 H213 110(3) no
C20 . C21 H211 109(3) no
H213 . C21 H211 109(4) no
C20 . C21 H212 113(3) no
H213 . C21 H212 107(4) no
H211 . C21 H212 109(4) no
C23 . C22 P2 116.6(2) yes
C23 . C22 H221 111(2) no
P2 . C22 H221 105(2) no
C23 . C22 H222 110(3) no
P2 . C22 H222 106(3) no
H221 . C22 H222 108(3) no
C22 . C23 H232 112(3) no
C22 . C23 H233 112(3) no
H232 . C23 H233 107(4) no
C22 . C23 H231 109(3) no
H232 . C23 H231 109(4) no
H233 . C23 H231 109(4) no
Rh1 2_576 Cl1 Rh1 99.30(3) yes
C15 . O1 C6 113.9(2) yes
C16 . P1 C18 101.50(15) yes
C16 . P1 C1 101.07(14) yes
C18 . P1 C1 103.32(15) yes
C16 . P1 Rh1 114.71(10) yes
C18 . P1 Rh1 122.95(11) yes
C1 . P1 Rh1 110.58(10) yes
C22 . P2 C20 100.46(15) yes
C22 . P2 C14 101.93(15) yes
C20 . P2 C14 102.45(14) yes
C22 . P2 Rh1 126.12(11) yes
C20 . P2 Rh1 112.67(11) yes
C14 . P2 Rh1 110.34(10) yes
Cl1 2_576 Rh1 Cl1 80.70(3) yes
Cl1 2_576 Rh1 P2 89.67(3) yes
Cl1 . Rh1 P2 169.68(3) yes
Cl1 2_576 Rh1 P1 169.89(3) yes
Cl1 . Rh1 P1 90.32(3) yes
P2 . Rh1 P1 98.96(3) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.407(4) yes
C1 C6 . 1.401(4) yes
C1 P1 . 1.834(3) yes
C2 C3 . 1.392(5) yes
C2 H21 . 1.00(4) no
C3 C4 . 1.395(5) yes
C3 H31 . 1.00(4) no
C4 C5 . 1.393(4) yes
C4 H41 . 0.98(4) no
C5 C6 . 1.387(4) yes
C5 C7 . 1.535(4) yes
C6 O1 . 1.380(4) yes
C7 C8 . 1.530(4) yes
C7 C9 . 1.543(4) yes
C7 C10 . 1.538(4) yes
C8 H81 . 1.02(5) no
C8 H83 . 0.99(5) no
C8 H82 . 1.01(5) no
C9 H92 . 0.95(5) no
C9 H91 . 1.00(5) no
C9 H93 . 1.01(5) no
C10 C11 . 1.397(4) yes
C10 C15 . 1.386(4) yes
C11 C12 . 1.392(5) yes
C11 H111 . 0.97(4) no
C12 C13 . 1.390(5) yes
C12 H121 . 0.95(4) no
C13 C14 . 1.399(4) yes
C13 H131 . 0.99(4) no
C14 C15 . 1.398(4) yes
C14 P2 . 1.834(3) yes
C15 O1 . 1.391(3) yes
C16 C17 . 1.522(5) yes
C16 P1 . 1.844(3) yes
C16 H162 . 0.98(4) no
C16 H161 . 0.99(4) no
C17 H172 . 1.02(5) no
C17 H171 . 1.01(5) no
C17 H173 . 0.98(5) no
C18 C19 . 1.521(4) yes
C18 P1 . 1.837(3) yes
C18 H181 . 0.98(4) no
C18 H182 . 0.92(4) no
C19 H191 . 1.00(5) no
C19 H193 . 0.98(5) no
C19 H192 . 1.00(5) no
C20 C21 . 1.527(5) yes
C20 P2 . 1.842(3) yes
C20 H202 . 0.97(4) no
C20 H201 . 1.01(4) no
C21 H213 . 1.01(5) no
C21 H211 . 1.01(5) no
C21 H212 . 0.97(5) no
C22 C23 . 1.532(5) yes
C22 P2 . 1.848(3) yes
C22 H221 . 1.01(4) no
C22 H222 . 0.94(4) no
C23 H232 . 0.99(5) no
C23 H233 . 1.05(5) no
C23 H231 . 1.02(5) no
Cl1 Rh1 2_576 2.4322(7) yes
Cl1 Rh1 . 2.4131(8) yes
P1 Rh1 . 2.2191(7) yes
P2 Rh1 . 2.2267(8) yes
