#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/12/4121222.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_4121222
loop_
_publ_author_name
'Markus G. Scheibel'
'Yanlin Wu'
'A. Claudia Stückl'
'Lennard Krause'
'Elena Carl'
'Dietmar Stalke'
'Bas de Bruin'
'Sven Schneider'
_publ_section_title
;
 Synthesis and Reactivity of a Transient, Terminal Nitrido Complex of
 Rhodium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17719
_journal_page_last               17722
_journal_paper_doi               10.1021/ja409764j
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C20 H40 N3 P2 Rh1'
_chemical_formula_sum            'C20 H40 N3 P2 Rh'
_chemical_formula_weight         487.4
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 106.53(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.867(2)
_cell_length_b                   27.050(6)
_cell_length_c                   11.866(2)
_cell_measurement_reflns_used    4429
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.7865
_cell_measurement_theta_min      2.2125
_cell_volume                     2420.8(9)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'shelXle v0.477'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Smart APEX II Ultra'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56085
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22081
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        19.665
_diffrn_reflns_theta_max         20.943
_diffrn_reflns_theta_min         1.188
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.5950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       neelde
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.041
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5218
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[σ²(Fo²)+(0.0454P)²+1.6943P]
 where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0920
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4288
_reflns_number_total             5218
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja409764j_si_003.cif
_cod_data_source_block           P21c_a
_cod_original_formula_sum        'C20 H40 N3 P2 Rh1'
_cod_database_code               4121222
#BEGIN Tags that were not found in dictionaries:
_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.
;
_shelxl_version_number           2012-6
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Rh1 Rh 0.68167(4) 0.87187(2) 0.61776(2) 0.01061(9) Uani 1 1 d . U
P1 P 0.84854(11) 0.90643(3) 0.79388(7) 0.01209(18) Uani 1 1 d . .
P2 P 0.48518(11) 0.85950(3) 0.43332(7) 0.01263(18) Uani 1 1 d . .
N1 N 0.5379(4) 0.93439(9) 0.6120(2) 0.0124(6) Uani 1 1 d . .
N2 N 0.8104(4) 0.81155(10) 0.6240(2) 0.0153(6) Uani 1 1 d . U
N3 N 0.8803(4) 0.77657(11) 0.6262(3) 0.0251(7) Uani 1 1 d . U
C1 C 0.5784(4) 0.96700(11) 0.7047(3) 0.0147(7) Uani 1 1 d . .
H1 H 0.5057 0.9953 0.7013 0.018 Uiso 1 1 calc R U
C2 C 0.7183(4) 0.96006(11) 0.8004(3) 0.0146(7) Uani 1 1 d . .
H2 H 0.7454 0.9819 0.8659 0.018 Uiso 1 1 calc R U
C3 C 1.0713(5) 0.92993(12) 0.7881(3) 0.0163(7) Uani 1 1 d . .
C4 C 1.0306(5) 0.96875(14) 0.6879(3) 0.0284(9) Uani 1 1 d . .
H4A H 1.1418 0.9800 0.6747 0.043 Uiso 1 1 calc R U
H4B H 0.9690 0.9970 0.7101 0.043 Uiso 1 1 calc R U
H4C H 0.9551 0.9538 0.6157 0.043 Uiso 1 1 calc R U
C5 C 1.1818(5) 0.95457(14) 0.9015(3) 0.0266(8) Uani 1 1 d . .
H5A H 1.2858 0.9705 0.8874 0.040 Uiso 1 1 calc R U
H5B H 1.2206 0.9295 0.9632 0.040 Uiso 1 1 calc R U
H5C H 1.1098 0.9795 0.9266 0.040 Uiso 1 1 calc R U
C6 C 1.1774(5) 0.88804(14) 0.7522(4) 0.0277(9) Uani 1 1 d . .
H6A H 1.1091 0.8744 0.6763 0.042 Uiso 1 1 calc R U
H6B H 1.2004 0.8619 0.8119 0.042 Uiso 1 1 calc R U
H6C H 1.2903 0.9011 0.7455 0.042 Uiso 1 1 calc R U
C7 C 0.8636(5) 0.87086(12) 0.9322(3) 0.0176(7) Uani 1 1 d . .
C8 C 0.9075(5) 0.90323(13) 1.0443(3) 0.0224(8) Uani 1 1 d . .
H8A H 1.0268 0.9171 1.0585 0.034 Uiso 1 1 calc R U
H8B H 0.9026 0.8829 1.1117 0.034 Uiso 1 1 calc R U
H8C H 0.8209 0.9301 1.0338 0.034 Uiso 1 1 calc R U
C9 C 0.6760(5) 0.84945(14) 0.9148(3) 0.0268(8) Uani 1 1 d . .
H9A H 0.5904 0.8766 0.9047 0.040 Uiso 1 1 calc R U
H9B H 0.6741 0.8299 0.9839 0.040 Uiso 1 1 calc R U
H9C H 0.6445 0.8283 0.8449 0.040 Uiso 1 1 calc R U
C10 C 0.9963(5) 0.82825(13) 0.9484(3) 0.0253(8) Uani 1 1 d . .
H10A H 0.9724 0.8091 0.8754 0.038 Uiso 1 1 calc R U
H10B H 0.9846 0.8068 1.0122 0.038 Uiso 1 1 calc R U
H10C H 1.1171 0.8416 0.9680 0.038 Uiso 1 1 calc R U
C11 C 0.3972(4) 0.94446(11) 0.5150(3) 0.0148(7) Uani 1 1 d . .
H11 H 0.3303 0.9737 0.5144 0.018 Uiso 1 1 calc R U
C12 C 0.3511(5) 0.91407(12) 0.4205(3) 0.0157(7) Uani 1 1 d . .
H12 H 0.2554 0.9211 0.3528 0.019 Uiso 1 1 calc R U
C13 C 0.5898(5) 0.86358(12) 0.3078(3) 0.0180(7) Uani 1 1 d . .
C14 C 0.7394(5) 0.90232(13) 0.3495(3) 0.0212(8) Uani 1 1 d . .
H14A H 0.7935 0.9088 0.2861 0.032 Uiso 1 1 calc R U
H14B H 0.8296 0.8896 0.4184 0.032 Uiso 1 1 calc R U
H14C H 0.6897 0.9330 0.3704 0.032 Uiso 1 1 calc R U
C15 C 0.4612(5) 0.88213(15) 0.1930(3) 0.0278(9) Uani 1 1 d . .
H15A H 0.5237 0.8849 0.1327 0.042 Uiso 1 1 calc R U
H15B H 0.4149 0.9146 0.2061 0.042 Uiso 1 1 calc R U
H15C H 0.3627 0.8587 0.1668 0.042 Uiso 1 1 calc R U
C16 C 0.6731(5) 0.81422(13) 0.2875(3) 0.0249(8) Uani 1 1 d . .
H16A H 0.5791 0.7902 0.2537 0.037 Uiso 1 1 calc R U
H16B H 0.7486 0.8017 0.3626 0.037 Uiso 1 1 calc R U
H16C H 0.7449 0.8193 0.2331 0.037 Uiso 1 1 calc R U
C17 C 0.3268(5) 0.80600(12) 0.4148(3) 0.0179(7) Uani 1 1 d . .
C18 C 0.2237(5) 0.81483(14) 0.5051(3) 0.0272(9) Uani 1 1 d . .
H18A H 0.1546 0.8454 0.4855 0.041 Uiso 1 1 calc R U
H18B H 0.3072 0.8178 0.5837 0.041 Uiso 1 1 calc R U
H18C H 0.1435 0.7870 0.5036 0.041 Uiso 1 1 calc R U
C19 C 0.1949(5) 0.80259(15) 0.2917(3) 0.0311(9) Uani 1 1 d . .
H19A H 0.2582 0.7933 0.2347 0.047 Uiso 1 1 calc R U
H19B H 0.1373 0.8347 0.2700 0.047 Uiso 1 1 calc R U
H19C H 0.1049 0.7776 0.2918 0.047 Uiso 1 1 calc R U
C20 C 0.4279(5) 0.75707(13) 0.4461(3) 0.0257(8) Uani 1 1 d . .
H20A H 0.3433 0.7301 0.4420 0.039 Uiso 1 1 calc R U
H20B H 0.5084 0.7591 0.5259 0.039 Uiso 1 1 calc R U
H20C H 0.4965 0.7508 0.3904 0.039 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 0.0015 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0667 0.0580 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -2.5280 0.5964 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
N2 Rh1 N1 177.93(11)
N2 Rh1 P2 96.73(8)
N1 Rh1 P2 82.69(8)
N2 Rh1 P1 98.68(8)
N1 Rh1 P1 82.04(8)
P2 Rh1 P1 164.12(3)
C2 P1 C7 105.79(15)
C2 P1 C3 106.13(15)
C7 P1 C3 112.13(16)
C2 P1 Rh1 100.44(11)
C7 P1 Rh1 117.32(11)
C3 P1 Rh1 113.35(11)
C12 P2 C17 105.60(16)
C12 P2 C13 105.12(15)
C17 P2 C13 111.92(15)
C12 P2 Rh1 100.33(11)
C17 P2 Rh1 117.61(11)
C13 P2 Rh1 114.28(12)
C1 N1 C11 119.3(3)
C1 N1 Rh1 120.6(2)
C11 N1 Rh1 120.1(2)
N3 N2 Rh1 178.3(3)
C2 C1 N1 122.1(3)
C1 C2 P1 114.5(2)
C5 C3 C6 110.3(3)
C5 C3 C4 108.7(3)
C6 C3 C4 107.3(3)
C5 C3 P1 114.6(2)
C6 C3 P1 110.2(2)
C4 C3 P1 105.4(2)
C10 C7 C9 109.0(3)
C10 C7 C8 109.9(3)
C9 C7 C8 107.3(3)
C10 C7 P1 111.6(2)
C9 C7 P1 104.8(2)
C8 C7 P1 113.9(2)
C12 C11 N1 122.3(3)
C11 C12 P2 114.6(3)
C15 C13 C16 110.4(3)
C15 C13 C14 108.2(3)
C16 C13 C14 108.6(3)
C15 C13 P2 113.1(2)
C16 C13 P2 111.8(2)
C14 C13 P2 104.4(2)
C20 C17 C19 110.0(3)
C20 C17 C18 107.8(3)
C19 C17 C18 108.9(3)
C20 C17 P2 110.8(2)
C19 C17 P2 113.8(3)
C18 C17 P2 105.2(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Rh1 N2 1.911(3)
Rh1 N1 2.025(3)
Rh1 P2 2.3165(10)
Rh1 P1 2.3246(10)
P1 C2 1.790(3)
P1 C7 1.876(3)
P1 C3 1.883(4)
P2 C12 1.796(3)
P2 C17 1.881(3)
P2 C13 1.899(3)
N1 C1 1.375(4)
N1 C11 1.378(4)
N2 N3 1.091(4)
C1 C2 1.351(5)
C3 C5 1.531(5)
C3 C6 1.538(5)
C3 C4 1.550(5)
C7 C10 1.530(5)
C7 C9 1.544(5)
C7 C8 1.548(4)
C11 C12 1.354(5)
C13 C15 1.531(5)
C13 C16 1.537(5)
C13 C14 1.548(5)
C17 C20 1.534(5)
C17 C19 1.535(5)
C17 C18 1.535(5)
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
C11 N1 C1 C2 -177.6(3)
Rh1 N1 C1 C2 2.7(4)
N1 C1 C2 P1 1.9(4)
C7 P1 C2 C1 -127.0(3)
C3 P1 C2 C1 113.7(3)
Rh1 P1 C2 C1 -4.5(3)
C2 P1 C3 C5 68.7(3)
C7 P1 C3 C5 -46.4(3)
Rh1 P1 C3 C5 177.9(2)
C2 P1 C3 C6 -166.2(2)
C7 P1 C3 C6 78.7(3)
Rh1 P1 C3 C6 -56.9(3)
C2 P1 C3 C4 -50.8(3)
C7 P1 C3 C4 -165.9(2)
Rh1 P1 C3 C4 58.5(2)
C2 P1 C7 C10 -170.7(2)
C3 P1 C7 C10 -55.5(3)
Rh1 P1 C7 C10 78.3(3)
C2 P1 C7 C9 71.4(3)
C3 P1 C7 C9 -173.4(2)
Rh1 P1 C7 C9 -39.6(3)
C2 P1 C7 C8 -45.6(3)
C3 P1 C7 C8 69.7(3)
Rh1 P1 C7 C8 -156.6(2)
C1 N1 C11 C12 179.5(3)
Rh1 N1 C11 C12 -0.9(4)
N1 C11 C12 P2 1.0(4)
C17 P2 C12 C11 122.0(3)
C13 P2 C12 C11 -119.5(3)
Rh1 P2 C12 C11 -0.7(3)
C12 P2 C13 C15 -40.9(3)
C17 P2 C13 C15 73.2(3)
Rh1 P2 C13 C15 -149.9(2)
C12 P2 C13 C16 -166.4(2)
C17 P2 C13 C16 -52.2(3)
Rh1 P2 C13 C16 84.6(3)
C12 P2 C13 C14 76.4(2)
C17 P2 C13 C14 -169.4(2)
Rh1 P2 C13 C14 -32.6(2)
C12 P2 C17 C20 -169.7(2)
C13 P2 C17 C20 76.5(3)
Rh1 P2 C17 C20 -58.8(3)
C12 P2 C17 C19 65.8(3)
C13 P2 C17 C19 -48.1(3)
Rh1 P2 C17 C19 176.6(2)
C12 P2 C17 C18 -53.4(3)
C13 P2 C17 C18 -167.3(2)
Rh1 P2 C17 C18 57.4(3)
