#------------------------------------------------------------------------------
#$Date: 2019-11-03 14:11:55 +0200 (Sun, 03 Nov 2019) $
#$Revision: 221612 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/85/4128530.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_4128530
loop_
_publ_author_name
'Kim, Jinwoo'
'Shin, Kwangmin'
'Jin, Seongho'
'Kim, Dongwook'
'Chang, Sukbok'
_publ_section_title
;
 Oxidatively Induced Reductive Elimination: Exploring the Scope and
 Catalyst Systems with Ir, Rh, and Ru Complexes.
;
_journal_issue                   9
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4137
_journal_page_last               4146
_journal_paper_doi               10.1021/jacs.9b00364
_journal_volume                  141
_journal_year                    2019
_chemical_formula_sum            'C24 H26 N Rh'
_chemical_formula_weight         431.37
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.7219(9)
_cell_length_b                   15.4380(18)
_cell_length_c                   16.476(2)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      29.26
_cell_measurement_theta_min      3.20
_cell_volume                     1964.1(4)
_computing_cell_refinement       'Bruker APEXIII'
_computing_data_collection       'Bruker APEXIII'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Photon 100 CMOS detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1067
_diffrn_reflns_av_unetI/netI     0.0695
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            59048
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.380
_diffrn_reflns_theta_min         2.913
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.876
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.7064
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.185
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.993
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0032(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3226
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1220
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0547P)²+4.8648P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1894
_reflns_number_total             3226
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b00364_si_005.cif
_cod_data_source_block           A044_062
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'MULTI-SCAN' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               4128530
_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.
;
_shelx_estimated_absorpt_t_min   0.855
_shelx_estimated_absorpt_t_max   0.945
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, 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
Rh1 Rh 0.74979(5) 0.250000 0.47621(2) 0.02895(17) Uani 1 2 d S T P A .
C1M C 1.0043(6) 0.250000 0.4193(3) 0.0283(11) Uani 1 2 d S T P A .
H1M1 H 1.029397 0.307877 0.397839 0.042 Uiso 0.5 1 calc R U P . .
H1M2 H 1.005915 0.207865 0.374783 0.042 Uiso 0.5 1 calc R U P . .
H1M3 H 1.092250 0.234258 0.459551 0.042 Uiso 0.5 1 calc R U P . .
N1 N 0.868(2) 0.1590(11) 0.5567(11) 0.024(3) Uani 0.5 1 d D . P A 1
C21 C 0.834(3) 0.0708(11) 0.5508(17) 0.039(4) Uani 0.5 1 d D . P A 1
H21 H 0.757575 0.046739 0.511807 0.046 Uiso 0.5 1 calc R U P A 1
C31 C 0.924(4) 0.0209(16) 0.6079(13) 0.073(6) Uani 0.5 1 d D U P A 1
H31 H 0.934690 -0.040238 0.603320 0.087 Uiso 0.5 1 calc R U P A 1
C41 C 0.997(3) 0.0672(7) 0.6720(12) 0.066(5) Uani 0.5 1 d D U P A 1
H41 H 1.043858 0.031686 0.713648 0.079 Uiso 0.5 1 calc R U P A 1
C1 C 0.839(3) 0.1708(15) 0.5588(13) 0.031(4) Uani 0.5 1 d D U P A 2
C22 C 0.872(3) 0.0823(14) 0.5617(16) 0.040(4) Uani 0.5 1 d D . P A 2
H22 H 0.848956 0.051791 0.512812 0.048 Uiso 0.5 1 calc R U P A 2
C32 C 0.933(3) 0.0313(12) 0.6257(12) 0.054(4) Uani 0.5 1 d D U P A 2
H32 H 0.916453 -0.029645 0.623968 0.064 Uiso 0.5 1 calc R U P A 2
C42 C 1.017(4) 0.0675(6) 0.6910(12) 0.061(5) Uani 0.5 1 d D U P A 2
H42 H 1.070209 0.035343 0.733410 0.074 Uiso 0.5 1 calc R U P A 2
C5 C 1.0145(5) 0.1567(4) 0.6868(3) 0.0603(16) Uani 1 1 d D . . . .
C6 C 0.9375(4) 0.2043(3) 0.6220(2) 0.0392(10) Uani 1 1 d D . . . .
C7 C 1.0861(6) 0.2072(5) 0.7516(3) 0.083(3) Uani 1 1 d . . . . .
H7 H 1.135721 0.177809 0.796633 0.100 Uiso 1 1 calc R U . . .
C8 C 0.6156(10) 0.250000 0.3579(4) 0.077(3) Uani 1 2 d S TU P A .
C9 C 0.5641(6) 0.1743(4) 0.4020(3) 0.0607(14) Uani 1 1 d . U . . .
C10 C 0.4750(5) 0.2041(3) 0.4718(3) 0.0415(10) Uani 1 1 d . U . . .
C11 C 0.7105(14) 0.250000 0.2779(5) 0.143(6) Uani 1 2 d S TU P . .
H11A H 0.730542 0.309849 0.260397 0.215 Uiso 0.5 1 calc R U P A .
H11B H 0.821858 0.220326 0.284198 0.215 Uiso 0.5 1 calc R U P . .
H11C H 0.640740 0.219826 0.236990 0.215 Uiso 0.5 1 calc R U P . .
C12 C 0.5752(11) 0.0819(6) 0.3747(6) 0.158(5) Uani 1 1 d . . . . .
H12A H 0.644007 0.078513 0.324853 0.238 Uiso 1 1 calc R U . . .
H12B H 0.630459 0.047102 0.417199 0.238 Uiso 1 1 calc R U . . .
H12C H 0.458434 0.059661 0.364325 0.238 Uiso 1 1 calc R U . . .
C13 C 0.3883(7) 0.1492(4) 0.5348(4) 0.083(2) Uani 1 1 d . . . . .
H13A H 0.406124 0.087886 0.521866 0.124 Uiso 1 1 calc R U . . .
H13B H 0.438097 0.161880 0.588220 0.124 Uiso 1 1 calc R U . . .
H13C H 0.263950 0.161879 0.535561 0.124 Uiso 1 1 calc R U . . .
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'
N N 0.0061 0.0033 '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
C1 Rh1 C1 77.5(8) 7_565 .
N1 Rh1 N1 82.2(5) . 7_565
C1 Rh1 C1M 89.0(9) 7_565 .
C1 Rh1 C1M 89.0(9) . .
N1 Rh1 C1M 83.2(6) . .
N1 Rh1 C1M 83.2(6) 7_565 .
C1 Rh1 C8 141.2(4) 7_565 .
C1 Rh1 C8 141.2(4) . .
N1 Rh1 C8 138.5(2) . .
N1 Rh1 C8 138.5(2) 7_565 .
C1M Rh1 C8 92.5(2) . .
C1 Rh1 C9 160.2(9) 7_565 .
C1 Rh1 C9 106.3(5) . .
N1 Rh1 C9 105.8(3) . .
N1 Rh1 C9 164.8(6) 7_565 .
C1M Rh1 C9 110.23(17) . .
C8 Rh1 C9 37.77(18) . .
N1 Rh1 C9 164.8(6) . 7_565
N1 Rh1 C9 105.8(3) 7_565 7_565
C1M Rh1 C9 110.23(17) . 7_565
C8 Rh1 C9 37.77(18) . 7_565
C9 Rh1 C9 63.6(3) . 7_565
C1 Rh1 C10 123.6(9) 7_565 .
C1 Rh1 C10 99.1(8) . .
N1 Rh1 C10 102.5(6) . .
N1 Rh1 C10 129.3(6) 7_565 .
C1M Rh1 C10 147.33(15) . .
C8 Rh1 C10 61.7(2) . .
C9 Rh1 C10 37.12(17) . .
C9 Rh1 C10 62.35(17) 7_565 .
C1 Rh1 C10 99.1(8) 7_565 7_565
C1 Rh1 C10 123.6(9) . 7_565
N1 Rh1 C10 129.3(6) . 7_565
N1 Rh1 C10 102.5(6) 7_565 7_565
C1M Rh1 C10 147.33(15) . 7_565
C8 Rh1 C10 61.7(2) . 7_565
C9 Rh1 C10 62.35(17) . 7_565
C9 Rh1 C10 37.11(17) 7_565 7_565
C10 Rh1 C10 36.9(2) . 7_565
C21 N1 C6 128.3(18) . .
C21 N1 Rh1 121.4(9) . .
C6 N1 Rh1 108.3(9) . .
N1 C21 C31 113.5(19) . .
C41 C31 C21 115(2) . .
C31 C41 C5 132.3(18) . .
C22 C1 C6 103.8(16) . .
C22 C1 Rh1 134.7(12) . .
C6 C1 Rh1 118.8(15) . .
C1 C22 C32 130(2) . .
C42 C32 C22 121.4(18) . .
C32 C42 C5 111.1(15) . .
C42 C5 C6 124.0(9) . .
C41 C5 C6 109.6(9) . .
C42 C5 C7 120.0(8) . .
C41 C5 C7 134.4(9) . .
C6 C5 C7 116.0(5) . .
N1 C6 C6 120.2(8) . 7_565
N1 C6 C5 118.7(9) . .
C1 C6 C5 126.7(11) . .
C6 C6 C5 121.0(3) 7_565 .
C7 C7 C5 123.0(3) 7_565 .
C9 C8 C9 109.4(6) . 7_565
C9 C8 C11 125.3(3) . .
C9 C8 C11 125.3(3) 7_565 .
C9 C8 Rh1 71.5(3) . .
C9 C8 Rh1 71.5(3) 7_565 .
C11 C8 Rh1 122.9(6) . .
C10 C9 C8 106.3(5) . .
C10 C9 C12 125.5(7) . .
C8 C9 C12 127.5(6) . .
C10 C9 Rh1 72.2(2) . .
C8 C9 Rh1 70.7(3) . .
C12 C9 Rh1 129.1(4) . .
C10 C10 C9 109.0(3) 7_565 .
C10 C10 C13 124.5(3) 7_565 .
C9 C10 C13 126.5(5) . .
C10 C10 Rh1 71.56(11) 7_565 .
C9 C10 Rh1 70.7(3) . .
C13 C10 Rh1 125.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 C1 1.95(2) 7_565
Rh1 C1 1.95(2) .
Rh1 N1 2.137(18) .
Rh1 N1 2.137(18) 7_565
Rh1 C1M 2.178(5) .
Rh1 C8 2.208(7) .
Rh1 C9 2.218(5) .
Rh1 C9 2.218(5) 7_565
Rh1 C10 2.238(4) .
Rh1 C10 2.238(4) 7_565
N1 C21 1.389(9) .
N1 C6 1.391(8) .
C21 C31 1.401(9) .
C31 C41 1.394(9) .
C41 C5 1.409(9) .
C1 C22 1.391(9) .
C1 C6 1.392(9) .
C22 C32 1.398(9) .
C32 C42 1.376(9) .
C42 C5 1.378(9) .
C5 C6 1.425(6) .
C5 C7 1.434(8) .
C6 C6 1.411(9) 7_565
C7 C7 1.322(14) 7_565
C8 C9 1.433(7) .
C8 C9 1.433(7) 7_565
C8 C11 1.508(12) .
C9 C10 1.418(7) .
C9 C12 1.497(9) .
C10 C10 1.416(9) 7_565
C10 C13 1.498(7) .
