#------------------------------------------------------------------------------
#$Date: 2022-03-05 01:57:10 +0200 (Sat, 05 Mar 2022) $
#$Revision: 273445 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/96/7709654.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_7709654
loop_
_publ_author_name
'Drescher, Wiebke'
'Kleeberg, Christian'
_publ_section_title
;
 Ligand properties of boryl ligands in bis-boryl rhodium(iii) complexes: a
 case study
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT04276A
_journal_year                    2022
_chemical_formula_moiety         'C21 H35 B2 Cl O4 P3 Rh'
_chemical_formula_sum            'C21 H35 B2 Cl O4 P3 Rh'
_chemical_formula_weight         604.38
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-12-20 deposited with the CCDC.	2022-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.003(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.98020(10)
_cell_length_b                   32.0928(6)
_cell_length_c                   9.3574(2)
_cell_measurement_reflns_used    90383
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.2540
_cell_measurement_theta_min      2.8630
_cell_volume                     2695.15(8)
_computing_cell_refinement
;
 CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2019.)
;
_computing_data_collection
;
 CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2019.)
;
_computing_data_reduction
;
 CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2019.)
;
_computing_molecular_graphics
;
 K. Brandenburg, 2017, Diamond 4.4.1, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material
;
 WinGX v2014.1 (L. J. Farrugia, J. Appl. Cryst., 2012, 45, 849-854.)
;
_computing_structure_refinement
;
 SHELXL-2018/3 (G. M. Sheldrick, Acta Cryst., 2015, C71, 3--8)
;
_computing_structure_solution
;
 SHELXT (Ver. 2014/5) (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0170
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            217706
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.080
_diffrn_reflns_theta_min         2.600
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.936
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.40.50a (Rigaku Oxford Diffraction, 2019)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.

 Empirical correction (ABSPACK) includes:
 - Absorption correction using spherical harmonics
 - Frame scaling
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_recrystallization_method
;
 Slow evaporation of a solution in C6D6 layered with n-pentane
 at ambient temperature.
;
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.441
_refine_diff_density_min         -1.771
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.172
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         11930
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0350P)²+1.5566P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10966
_reflns_number_total             11930
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt04276a2.cif
_cod_data_source_block           wo100wo
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7709654
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.49710(14) 0.57719(4) 0.26416(14) 0.0153(2) Uani 1 1 d . . . . .
C2 C 0.40894(14) 0.61247(4) 0.25289(14) 0.0173(2) Uani 1 1 d . . . . .
C3 C 0.28398(17) 0.61412(6) 0.16256(17) 0.0258(3) Uani 1 1 d . . . . .
H3 H 0.224244 0.638485 0.154328 0.031 Uiso 1 1 calc R U . . .
C4 C 0.24981(17) 0.57800(6) 0.08370(17) 0.0269(3) Uani 1 1 d . . . . .
H4 H 0.164856 0.577850 0.020284 0.032 Uiso 1 1 calc R U . . .
C5 C 0.33752(18) 0.54244(5) 0.09629(17) 0.0245(3) Uani 1 1 d . . . . .
H5 H 0.310837 0.518405 0.041960 0.029 Uiso 1 1 calc R U . . .
C6 C 0.46485(17) 0.54133(5) 0.18774(15) 0.0209(2) Uani 1 1 d . . . . .
H6 H 0.525582 0.517168 0.196546 0.025 Uiso 1 1 calc R U . . .
C7 C 0.97955(15) 0.55430(4) 0.69542(15) 0.0178(2) Uani 1 1 d . . . . .
C8 C 1.03638(14) 0.56149(4) 0.56231(15) 0.0161(2) Uani 1 1 d . . . . .
C9 C 1.14790(15) 0.53724(4) 0.50789(17) 0.0205(2) Uani 1 1 d . . . . .
H9 H 1.187624 0.542598 0.416930 0.025 Uiso 1 1 calc R U . . .
C10 C 1.19920(16) 0.50426(5) 0.59438(19) 0.0241(3) Uani 1 1 d . . . . .
H10 H 1.275299 0.486562 0.560956 0.029 Uiso 1 1 calc R U . . .
C11 C 1.14163(17) 0.49679(5) 0.72777(19) 0.0256(3) Uani 1 1 d . . . . .
H11 H 1.179175 0.474112 0.783441 0.031 Uiso 1 1 calc R U . . .
C12 C 1.02931(18) 0.52198(5) 0.78209(17) 0.0236(3) Uani 1 1 d . . . . .
H12 H 0.989631 0.517094 0.873383 0.028 Uiso 1 1 calc R U . . .
C13 C 0.85625(16) 0.64648(5) 0.22438(14) 0.0195(2) Uani 1 1 d . . . . .
H13A H 0.754602 0.645498 0.182866 0.029 Uiso 1 1 calc R U . . .
H13B H 0.888965 0.618215 0.249714 0.029 Uiso 1 1 calc R U . . .
H13C H 0.923273 0.658289 0.154548 0.029 Uiso 1 1 calc R U . . .
C14 C 1.06119(14) 0.68363(4) 0.41565(15) 0.0178(2) Uani 1 1 d . . . . .
H14A H 1.105443 0.696467 0.332123 0.027 Uiso 1 1 calc R U . . .
H14B H 1.104426 0.655903 0.431555 0.027 Uiso 1 1 calc R U . . .
H14C H 1.081639 0.701045 0.500088 0.027 Uiso 1 1 calc R U . . .
C15 C 0.80692(16) 0.72923(4) 0.30975(15) 0.0197(2) Uani 1 1 d . . . . .
H15A H 0.874683 0.736645 0.233938 0.030 Uiso 1 1 calc R U . . .
H15B H 0.812861 0.750404 0.385183 0.030 Uiso 1 1 calc R U . . .
H15C H 0.704662 0.727792 0.269902 0.030 Uiso 1 1 calc R U . . .
C16 C 0.89275(16) 0.75229(4) 0.68612(15) 0.0184(2) Uani 1 1 d . . . . .
H16A H 0.805212 0.765974 0.641763 0.028 Uiso 1 1 calc R U . . .
H16B H 0.970730 0.749841 0.615906 0.028 Uiso 1 1 calc R U . . .
H16C H 0.929999 0.768876 0.767709 0.028 Uiso 1 1 calc R U . . .
C17 C 1.01288(15) 0.68148(5) 0.83538(16) 0.0195(2) Uani 1 1 d . . . . .
H17A H 1.046138 0.701372 0.909267 0.029 Uiso 1 1 calc R U . . .
H17B H 1.090021 0.678616 0.764497 0.029 Uiso 1 1 calc R U . . .
H17C H 0.994758 0.654328 0.879463 0.029 Uiso 1 1 calc R U . . .
C18 C 0.73179(15) 0.71543(4) 0.90021(14) 0.0176(2) Uani 1 1 d . . . . .
H18A H 0.724276 0.691750 0.965690 0.026 Uiso 1 1 calc R U . . .
H18B H 0.631748 0.723869 0.866469 0.026 Uiso 1 1 calc R U . . .
H18C H 0.780709 0.738784 0.950336 0.026 Uiso 1 1 calc R U . . .
C19 C 0.6049(2) 0.61560(6) 0.90948(17) 0.0324(4) Uani 1 1 d . . . . .
H19A H 0.584725 0.641526 0.960643 0.049 Uiso 1 1 calc R U . . .
H19B H 0.711021 0.608763 0.920721 0.049 Uiso 1 1 calc R U . . .
H19C H 0.545557 0.592974 0.948822 0.049 Uiso 1 1 calc R U . . .
C20 C 0.3710(2) 0.64478(7) 0.7259(3) 0.0402(5) Uani 1 1 d . . . . .
H20A H 0.308729 0.627679 0.786780 0.060 Uiso 1 1 calc R U . . .
H20B H 0.326279 0.645827 0.628965 0.060 Uiso 1 1 calc R U . . .
H20C H 0.378216 0.673063 0.765028 0.060 Uiso 1 1 calc R U . . .
C21 C 0.5093(2) 0.56842(5) 0.67548(19) 0.0299(3) Uani 1 1 d . . . . .
H21A H 0.440433 0.557367 0.745103 0.045 Uiso 1 1 calc R U . . .
H21B H 0.600427 0.551616 0.677579 0.045 Uiso 1 1 calc R U . . .
H21C H 0.462027 0.567335 0.579541 0.045 Uiso 1 1 calc R U . . .
B1 B 0.59343(15) 0.62555(4) 0.41410(14) 0.0130(2) Uani 1 1 d . . . . .
B2 B 0.85500(15) 0.60838(4) 0.59556(15) 0.0137(2) Uani 1 1 d . . . . .
Cl1 Cl 0.54510(3) 0.71956(2) 0.55216(3) 0.01498(5) Uani 1 1 d . . . . .
O1 O 0.61317(11) 0.58464(3) 0.36150(11) 0.01670(17) Uani 1 1 d . . . . .
O2 O 0.46606(11) 0.64278(3) 0.34296(11) 0.01820(18) Uani 1 1 d . . . . .
O3 O 0.86847(11) 0.58295(3) 0.71976(11) 0.01829(18) Uani 1 1 d . . . . .
O4 O 0.96149(11) 0.59446(3) 0.49872(11) 0.01588(16) Uani 1 1 d . . . . .
P1 P 0.85981(4) 0.67889(2) 0.38428(3) 0.01284(6) Uani 1 1 d . . . . .
P2 P 0.84103(3) 0.70031(2) 0.74771(3) 0.01214(5) Uani 1 1 d . . . . .
P3 P 0.55546(4) 0.62217(2) 0.72045(4) 0.01419(6) Uani 1 1 d . . . . .
Rh1 Rh 0.71552(2) 0.65681(2) 0.57037(2) 0.00985(3) 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'
O O 0.0106 0.0060 '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'
Rh Rh -1.1178 0.9187 '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
C6 C1 O1 128.75(13) . . ?
C6 C1 C2 122.25(12) . . ?
O1 C1 C2 108.99(11) . . ?
O2 C2 C3 128.72(13) . . ?
O2 C2 C1 109.39(11) . . ?
C3 C2 C1 121.89(13) . . ?
C2 C3 C4 116.64(15) . . ?
C5 C4 C3 121.42(14) . . ?
C4 C5 C6 121.30(14) . . ?
C1 C6 C5 116.49(14) . . ?
O3 C7 C12 128.58(14) . . ?
O3 C7 C8 109.21(11) . . ?
C12 C7 C8 122.18(13) . . ?
O4 C8 C9 128.58(13) . . ?
O4 C8 C7 109.12(11) . . ?
C9 C8 C7 122.28(13) . . ?
C8 C9 C10 116.19(15) . . ?
C11 C10 C9 121.65(14) . . ?
C10 C11 C12 121.44(14) . . ?
C7 C12 C11 116.24(15) . . ?
O1 B1 O2 107.93(10) . . ?
O1 B1 Rh1 128.99(9) . . ?
O2 B1 Rh1 123.05(9) . . ?
O4 B2 O3 107.62(11) . . ?
O4 B2 Rh1 127.15(9) . . ?
O3 B2 Rh1 125.17(10) . . ?
C1 O1 B1 106.80(10) . . ?
C2 O2 B1 106.86(10) . . ?
C7 O3 B2 106.77(11) . . ?
C8 O4 B2 107.28(10) . . ?
C15 P1 C13 101.28(7) . . ?
C15 P1 C14 103.39(7) . . ?
C13 P1 C14 99.69(7) . . ?
C15 P1 Rh1 114.51(5) . . ?
C13 P1 Rh1 116.64(5) . . ?
C14 P1 Rh1 118.73(5) . . ?
C17 P2 C18 101.87(7) . . ?
C17 P2 C16 102.92(7) . . ?
C18 P2 C16 98.81(6) . . ?
C17 P2 Rh1 118.94(5) . . ?
C18 P2 Rh1 116.09(5) . . ?
C16 P2 Rh1 115.32(5) . . ?
C20 P3 C21 100.66(10) . . ?
C20 P3 C19 102.18(11) . . ?
C21 P3 C19 99.25(9) . . ?
C20 P3 Rh1 114.24(6) . . ?
C21 P3 Rh1 117.00(6) . . ?
C19 P3 Rh1 120.45(6) . . ?
B2 Rh1 B1 91.19(6) . . ?
B2 Rh1 P1 87.82(4) . . ?
B1 Rh1 P1 85.02(4) . . ?
B2 Rh1 P3 87.43(4) . . ?
B1 Rh1 P3 82.58(4) . . ?
P1 Rh1 P3 166.617(13) . . ?
B2 Rh1 P2 95.32(4) . . ?
B1 Rh1 P2 173.47(4) . . ?
P1 Rh1 P2 94.573(12) . . ?
P3 Rh1 P2 98.320(12) . . ?
B2 Rh1 Cl1 176.72(4) . . ?
B1 Rh1 Cl1 91.96(4) . . ?
P1 Rh1 Cl1 93.371(11) . . ?
P3 Rh1 Cl1 92.063(11) . . ?
P2 Rh1 Cl1 81.551(11) . . ?
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 C6 1.3804(19) . ?
C1 O1 1.3809(15) . ?
C1 C2 1.3833(19) . ?
C2 O2 1.3746(16) . ?
C2 C3 1.3821(19) . ?
C3 C4 1.402(2) . ?
C4 C5 1.389(3) . ?
C5 C6 1.405(2) . ?
C7 O3 1.3813(16) . ?
C7 C12 1.3814(19) . ?
C7 C8 1.382(2) . ?
C8 O4 1.3775(15) . ?
C8 C9 1.3799(19) . ?
C9 C10 1.400(2) . ?
C10 C11 1.388(3) . ?
C11 C12 1.402(2) . ?
C13 P1 1.8216(14) . ?
C14 P1 1.8282(13) . ?
C15 P1 1.8162(14) . ?
C16 P2 1.8300(14) . ?
C17 P2 1.8252(13) . ?
C18 P2 1.8253(13) . ?
C19 P3 1.8209(16) . ?
C20 P3 1.8107(17) . ?
C21 P3 1.8199(16) . ?
B1 O1 1.4153(17) . ?
B1 O2 1.4156(16) . ?
B1 Rh1 2.0579(14) . ?
B2 O4 1.4127(17) . ?
B2 O3 1.4218(17) . ?
B2 Rh1 2.0049(14) . ?
Cl1 Rh1 2.5315(3) . ?
P1 Rh1 2.3176(3) . ?
P2 Rh1 2.4171(3) . ?
P3 Rh1 2.3271(3) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C6 C1 C2 O2 178.74(13) . . . . ?
O1 C1 C2 O2 -0.43(15) . . . . ?
C6 C1 C2 C3 -0.9(2) . . . . ?
O1 C1 C2 C3 179.89(14) . . . . ?
O2 C2 C3 C4 -178.95(15) . . . . ?
C1 C2 C3 C4 0.7(2) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C3 C4 C5 C6 -0.5(3) . . . . ?
O1 C1 C6 C5 179.43(14) . . . . ?
C2 C1 C6 C5 0.4(2) . . . . ?
C4 C5 C6 C1 0.3(2) . . . . ?
O3 C7 C8 O4 -0.74(15) . . . . ?
C12 C7 C8 O4 177.47(13) . . . . ?
O3 C7 C8 C9 -179.09(12) . . . . ?
C12 C7 C8 C9 -0.9(2) . . . . ?
O4 C8 C9 C10 -177.00(13) . . . . ?
C7 C8 C9 C10 1.0(2) . . . . ?
C8 C9 C10 C11 -0.6(2) . . . . ?
C9 C10 C11 C12 0.0(2) . . . . ?
O3 C7 C12 C11 178.07(14) . . . . ?
C8 C7 C12 C11 0.2(2) . . . . ?
C10 C11 C12 C7 0.2(2) . . . . ?
C6 C1 O1 B1 -177.73(14) . . . . ?
C2 C1 O1 B1 1.37(14) . . . . ?
O2 B1 O1 C1 -1.79(14) . . . . ?
Rh1 B1 O1 C1 176.09(10) . . . . ?
C3 C2 O2 B1 178.96(16) . . . . ?
C1 C2 O2 B1 -0.70(15) . . . . ?
O1 B1 O2 C2 1.53(14) . . . . ?
Rh1 B1 O2 C2 -176.50(9) . . . . ?
C12 C7 O3 B2 -177.16(15) . . . . ?
C8 C7 O3 B2 0.90(15) . . . . ?
O4 B2 O3 C7 -0.73(14) . . . . ?
Rh1 B2 O3 C7 -177.99(10) . . . . ?
C9 C8 O4 B2 178.48(13) . . . . ?
C7 C8 O4 B2 0.26(14) . . . . ?
O3 B2 O4 C8 0.30(14) . . . . ?
Rh1 B2 O4 C8 177.49(10) . . . . ?
