#------------------------------------------------------------------------------
#$Date: 2019-11-07 23:17:02 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223978 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/01/7700110.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_7700110
loop_
_publ_author_name
'Lionetti, Davide'
'Day, Victor W.'
'Blakemore, James D.'
_publ_section_title
;
 Structural and chemical properties of half-sandwich rhodium complexes
 supported by the bis(2-pyridyl)methane ligand.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12396
_journal_page_last               12406
_journal_paper_doi               10.1039/c9dt01821b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '4(C23 H28 N3 Rh), 8(F6 P)'
_chemical_formula_sum            'C92 H112 F48 N12 P8 Rh4'
_chemical_formula_weight         2957.33
_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'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-29 deposited with the CCDC.    2019-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   16.7908(7)
_cell_length_b                   15.7747(6)
_cell_length_c                   10.9869(5)
_cell_measurement_reflns_used    8248
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      70.286
_cell_measurement_theta_min      4.810
_cell_volume                     2910.1(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      199.99
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker MicroStar microfocus rotating anode'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0908
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            26516
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        66.000
_diffrn_reflns_theta_max         70.510
_diffrn_reflns_theta_min         4.810
_diffrn_source                   'microfocus rotating anode generator'
_diffrn_source_type              'Bruker MicroStar'
_exptl_absorpt_coefficient_mu    6.686
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.4095
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1293 before and 0.0653 after correction. The Ratio of minimum to maximum transmission is 0.5436. The λ/2 correction factor is 0.00150.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.687
_exptl_crystal_description       prism
_exptl_crystal_F_000             1480
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile, diethyl ether'
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.468
_refine_diff_density_min         -0.662
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0350
_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)+(0.0351P)²+4.5288P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0867
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2517
_reflns_number_total             2850
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt01821b2.cif
_cod_data_source_block           1-NCCH3
_cod_depositor_comments
'Adding full bibliography for 7700110--7700111.cif.'
_cod_database_code               7700110
_shelx_shelxl_version_number     2014/7
_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_max   0.776
_shelx_estimated_absorpt_t_min   0.501
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H10A(0.5) H10B(0.5) H10C(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 F6(0.5) F7(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
3.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,
 H14C)
;
_olex2_submission_special_instructions 'No special instructions were received'
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 0.44478(2) 0.2500 0.35906(3) 0.02291(12) Uani 1 2 d S T P . .
N1 N 0.35278(15) 0.34059(17) 0.3529(2) 0.0309(5) Uani 1 1 d . . . . .
N3 N 0.4456(2) 0.2500 0.1698(3) 0.0319(8) Uani 1 2 d S T P . .
C1 C 0.3629(2) 0.4134(2) 0.2893(3) 0.0383(7) Uani 1 1 d . . . . .
H1 H 0.4082 0.4189 0.2380 0.046 Uiso 1 1 calc R . . . .
C2 C 0.3097(2) 0.4796(2) 0.2967(4) 0.0492(9) Uani 1 1 d . . . . .
H2 H 0.3181 0.5299 0.2509 0.059 Uiso 1 1 calc R . . . .
C3 C 0.2442(2) 0.4721(3) 0.3713(4) 0.0528(10) Uani 1 1 d . . . . .
H3 H 0.2077 0.5177 0.3801 0.063 Uiso 1 1 calc R . . . .
C4 C 0.2325(2) 0.3967(2) 0.4333(4) 0.0444(8) Uani 1 1 d . . . . .
H4 H 0.1867 0.3897 0.4830 0.053 Uiso 1 1 calc R . . . .
C5 C 0.28720(18) 0.3313(2) 0.4233(3) 0.0331(7) Uani 1 1 d . . . . .
C6 C 0.2779(3) 0.2500 0.4931(5) 0.0398(11) Uani 1 2 d S T P . .
H6A H 0.3174 0.2500 0.5600 0.048 Uiso 1 2 calc RS T P . .
H6B H 0.2244 0.2500 0.5310 0.048 Uiso 1 2 calc RS T P . .
C7 C 0.5742(2) 0.2500 0.3680(4) 0.0297(9) Uani 1 2 d S T P . .
C8 C 0.54280(17) 0.17656(18) 0.4263(3) 0.0291(6) Uani 1 1 d . . . . .
C9 C 0.49551(18) 0.20476(19) 0.5284(3) 0.0285(6) Uani 1 1 d . . . . .
C10 C 0.6300(3) 0.2500 0.2635(5) 0.0469(12) Uani 1 2 d S T P . .
H10A H 0.6129 0.2923 0.2037 0.070 Uiso 0.5 1 calc GR . . A -1
H10B H 0.6304 0.1938 0.2256 0.070 Uiso 0.5 1 calc GR . . A -1
H10C H 0.6837 0.2639 0.2921 0.070 Uiso 0.5 1 calc GR . . A -1
C11 C 0.5635(2) 0.0860(2) 0.3997(4) 0.0422(8) Uani 1 1 d . . . . .
H11A H 0.5777 0.0803 0.3135 0.063 Uiso 1 1 calc GR . . . .
H11B H 0.5176 0.0498 0.4178 0.063 Uiso 1 1 calc GR . . . .
H11C H 0.6088 0.0688 0.4503 0.063 Uiso 1 1 calc GR . . . .
C12 C 0.4576(2) 0.1481(2) 0.6208(3) 0.0404(8) Uani 1 1 d . . . . .
H12A H 0.4188 0.1805 0.6685 0.061 Uiso 1 1 calc GR . . . .
H12B H 0.4987 0.1254 0.6752 0.061 Uiso 1 1 calc GR . . . .
H12C H 0.4305 0.1012 0.5794 0.061 Uiso 1 1 calc GR . . . .
C13 C 0.4545(3) 0.2500 0.0683(4) 0.0331(10) Uani 1 2 d S T P . .
C14 C 0.4678(4) 0.2500 -0.0623(5) 0.0542(15) Uani 1 2 d S T P . .
H14A H 0.5197 0.2757 -0.0800 0.081 Uiso 0.5 1 calc GR . . B -1
H14B H 0.4257 0.2827 -0.1024 0.081 Uiso 0.5 1 calc GR . . B -1
H14C H 0.4671 0.1916 -0.0926 0.081 Uiso 0.5 1 calc GR . . B -1
P2 P 0.72362(9) 0.2500 0.66083(14) 0.0521(4) Uani 1 2 d S T P . .
F4 F 0.6732(3) 0.3195(2) 0.5947(4) 0.139(2) Uani 1 1 d . . . . .
F5 F 0.7729(3) 0.3179(2) 0.7309(4) 0.1284(18) Uani 1 1 d . . . . .
F6 F 0.7804(5) 0.2834(6) 0.5575(6) 0.130(4) Uani 0.5 1 d . . . C 2
F7 F 0.6662(4) 0.2753(5) 0.7668(7) 0.110(3) Uani 0.5 1 d . . . C 2
P1 P 0.5000 0.0000 0.0000 0.0329(3) Uani 1 2 d S T P . .
F1 F 0.46498(15) -0.07328(16) -0.0840(3) 0.0671(7) Uani 1 1 d . . . . .
F2 F 0.41956(14) 0.05230(16) -0.0084(3) 0.0649(7) Uani 1 1 d . . . . .
F3 F 0.5340(2) 0.04748(19) -0.1159(3) 0.0834(9) 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 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh 0.0927 3.6045 '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
N1 Rh1 N1 85.49(15) 7_565 .
N1 Rh1 C7 137.26(7) 7_565 .
N1 Rh1 C7 137.26(7) . .
N1 Rh1 C8 160.23(11) 7_565 7_565
N1 Rh1 C8 101.98(11) . 7_565
N1 Rh1 C8 160.23(11) . .
N1 Rh1 C8 101.98(11) 7_565 .
N1 Rh1 C9 95.31(11) . 7_565
N1 Rh1 C9 122.66(11) 7_565 7_565
N1 Rh1 C9 95.31(11) 7_565 .
N1 Rh1 C9 122.65(11) . .
N3 Rh1 N1 88.44(10) . 7_565
N3 Rh1 N1 88.44(10) . .
N3 Rh1 C7 92.19(16) . .
N3 Rh1 C8 109.85(12) . 7_565
N3 Rh1 C8 109.85(12) . .
N3 Rh1 C9 148.85(11) . .
N3 Rh1 C9 148.85(11) . 7_565
C8 Rh1 C7 38.53(10) . .
C8 Rh1 C7 38.53(10) 7_565 .
C8 Rh1 C8 65.42(16) . 7_565
C8 Rh1 C9 39.14(12) 7_565 7_565
C8 Rh1 C9 65.19(11) . 7_565
C8 Rh1 C9 65.19(11) 7_565 .
C8 Rh1 C9 39.14(12) . .
C9 Rh1 C7 64.45(14) 7_565 .
C9 Rh1 C7 64.45(14) . .
C9 Rh1 C9 38.45(16) . 7_565
C1 N1 Rh1 120.0(2) . .
C5 N1 Rh1 120.3(2) . .
C5 N1 C1 119.3(3) . .
C13 N3 Rh1 172.8(4) . .
N1 C1 H1 119.0 . .
N1 C1 C2 122.1(3) . .
C2 C1 H1 119.0 . .
C1 C2 H2 120.4 . .
C1 C2 C3 119.2(4) . .
C3 C2 H2 120.4 . .
C2 C3 H3 120.7 . .
C2 C3 C4 118.7(3) . .
C4 C3 H3 120.7 . .
C3 C4 H4 119.8 . .
C3 C4 C5 120.5(3) . .
C5 C4 H4 119.8 . .
N1 C5 C4 120.3(3) . .
N1 C5 C6 118.0(3) . .
C4 C5 C6 121.7(3) . .
C5 C6 C5 117.2(4) 7_565 .
C5 C6 H6A 108.0 7_565 .
C5 C6 H6A 108.0 . .
C5 C6 H6B 108.0 7_565 .
C5 C6 H6B 108.0 . .
H6A C6 H6B 107.2 . .
C8 C7 Rh1 69.5(2) . .
C8 C7 Rh1 69.5(2) 7_565 .
C8 C7 C8 108.7(4) . 7_565
C8 C7 C10 125.64(19) 7_565 .
C8 C7 C10 125.64(19) . .
C10 C7 Rh1 126.6(3) . .
C7 C8 Rh1 71.94(19) . .
C7 C8 C9 107.6(3) . .
C7 C8 C11 126.9(3) . .
C9 C8 Rh1 71.28(16) . .
C9 C8 C11 125.0(3) . .
C11 C8 Rh1 128.7(2) . .
C8 C9 Rh1 69.57(16) . .
C8 C9 C12 125.2(3) . .
C9 C9 Rh1 70.77(8) 7_565 .
C9 C9 C8 107.94(17) 7_565 .
C9 C9 C12 126.73(18) 7_565 .
C12 C9 Rh1 127.8(2) . .
C7 C10 H10A 109.5 . .
C7 C10 H10B 109.5 . .
C7 C10 H10C 109.5 . .
H10A C10 H10B 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C8 C11 H11A 109.5 . .
C8 C11 H11B 109.5 . .
C8 C11 H11C 109.5 . .
H11A C11 H11B 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C9 C12 H12A 109.5 . .
C9 C12 H12B 109.5 . .
C9 C12 H12C 109.5 . .
H12A C12 H12B 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N3 C13 C14 178.8(6) . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
F4 P2 F4 89.0(3) . 7_565
F4 P2 F6 76.0(4) 7_565 7_565
F4 P2 F6 103.1(4) . 7_565
F4 P2 F6 76.0(4) . .
F4 P2 F6 103.1(4) 7_565 .
F4 P2 F7 101.0(4) . 7_565
F4 P2 F7 101.0(4) 7_565 .
F4 P2 F7 80.4(4) . .
F4 P2 F7 80.4(4) 7_565 7_565
F5 P2 F4 92.01(17) . .
F5 P2 F4 92.01(17) 7_565 7_565
F5 P2 F4 178.1(3) . 7_565
F5 P2 F4 178.1(3) 7_565 .
F5 P2 F5 86.9(2) . 7_565
F5 P2 F6 105.4(4) . 7_565
F5 P2 F6 78.7(4) . .
F5 P2 F6 78.7(4) 7_565 7_565
F5 P2 F6 105.4(4) 7_565 .
F5 P2 F7 77.5(4) . .
F5 P2 F7 97.8(3) . 7_565
F5 P2 F7 77.5(4) 7_565 7_565
F5 P2 F7 97.8(3) 7_565 .
F6 P2 F6 39.1(7) . 7_565
F7 P2 F6 175.2(4) 7_565 .
F7 P2 F6 175.2(4) . 7_565
F7 P2 F6 145.6(5) . .
F7 P2 F6 145.6(5) 7_565 7_565
F7 P2 F7 29.6(6) 7_565 .
F6 F6 P2 70.4(3) 7_565 .
F7 F7 P2 75.2(3) 7_565 .
F1 P1 F1 180.0 5_655 .
F2 P1 F1 91.68(13) 5_655 5_655
F2 P1 F1 91.68(13) . .
F2 P1 F1 88.32(13) 5_655 .
F2 P1 F1 88.32(13) . 5_655
F2 P1 F2 180.0 5_655 .
F3 P1 F1 89.41(17) . 5_655
F3 P1 F1 89.41(17) 5_655 .
F3 P1 F1 90.59(17) . .
F3 P1 F1 90.59(17) 5_655 5_655
F3 P1 F2 90.81(17) 5_655 5_655
F3 P1 F2 89.19(17) 5_655 .
F3 P1 F2 90.81(17) . .
F3 P1 F2 89.19(17) . 5_655
F3 P1 F3 180.00(12) 5_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Rh1 N1 2.106(3) 7_565
Rh1 N1 2.106(3) .
Rh1 N3 2.080(4) .
Rh1 C7 2.176(4) .
Rh1 C8 2.144(3) 7_565
Rh1 C8 2.144(3) .
Rh1 C9 2.167(3) 7_565
Rh1 C9 2.167(3) .
N1 C1 1.355(4) .
N1 C5 1.354(4) .
N3 C13 1.125(6) .
C1 H1 0.9500 .
C1 C2 1.377(5) .
C2 H2 0.9500 .
C2 C3 1.377(6) .
C3 H3 0.9500 .
C3 C4 1.384(6) .
C4 H4 0.9500 .
C4 C5 1.385(5) .
C5 C6 1.503(4) .
C6 C5 1.503(4) 7_565
C6 H6A 0.9900 .
C6 H6B 0.9900 .
C7 C8 1.426(4) .
C7 C8 1.426(4) 7_565
C7 C10 1.482(6) .
C8 C9 1.444(4) .
C8 C11 1.499(4) .
C9 C9 1.427(6) 7_565
C9 C12 1.495(4) .
C10 H10A 0.9800 .
C10 H10B 0.9800 .
C10 H10C 0.9800 .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 C14 1.452(7) .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
P2 F4 1.563(3) .
P2 F4 1.563(3) 7_565
P2 F5 1.558(3) .
P2 F5 1.558(3) 7_565
P2 F6 1.574(7) .
P2 F6 1.574(7) 7_565
P2 F7 1.564(7) .
P2 F7 1.564(7) 7_565
F6 F6 1.053(18) 7_565
F7 F7 0.799(16) 7_565
P1 F1 1.592(2) 5_655
P1 F1 1.592(2) .
P1 F2 1.585(2) 5_655
P1 F2 1.585(2) .
P1 F3 1.584(3) 5_655
P1 F3 1.584(3) .
