Crystal structure of chlorido-(η 5-pentamethylcyclopentadienyl)-(4-chloro-4-pyridyl-2,2′:6′,2′′-terpyridine-κ2N,N′) rhodium(III) hexaflourophosphate, C31H29Cl2F6N3PRh
Gichumbi, Joel M.; Zamisa, Sizwe J.; Friedrich, Holger B.; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1403–1405; doi:10.1515/ncrs-2020-0337

data_8105478
_publ_section_title
;
 Crystal structure of chlorido-(\h
 5-pentamethylcyclopentadienyl)-(4-chloro-4-pyridyl-2,2&#x2032;:6&#x2032;,2&#x2032;&#x2032;-terpyridine-\k2N,N&#x2032;)
 rhodium(III) hexaflourophosphate, C31H29Cl2F6N3PRh
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1403
_journal_page_last               1405
_journal_paper_doi               10.1515/ncrs-2020-0337
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C31 H29 Cl2 N3 Rh, 1(F6 P)'
_chemical_formula_sum            'C31 H29 Cl2 F6 N3 P Rh'
_chemical_formula_weight         762.35
_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
_cell_angle_alpha                90
_cell_angle_beta                 93.924(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.4069(7)
_cell_length_b                   13.2451(12)
_cell_length_c                   32.141(3)
_cell_measurement_reflns_used    9949
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      26.20
_cell_measurement_theta_min      2.45
_cell_volume                     3145.8(5)
_computing_cell_refinement       'COSMO (Bruker, V1.61, 2009)'
_computing_data_collection       'COSMO (Bruker, V1.61, 2009)'
_computing_data_reduction        'SAINT (Bruker)'
_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    'ShelXS-2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture Diffractometer'
_diffrn_measurement_method       '1\% \f scans and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0863
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            106148
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.379
_diffrn_reflns_theta_min         1.270
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       block
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.728
_refine_diff_density_min         -0.587
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     462
_refine_ls_number_reflns         7840
_refine_ls_number_restraints     675
_refine_ls_restrained_S_all      1.163
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0386
_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/[\s^2^(Fo^2^)+(0.0386P)^2^+4.1560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0962
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6280
_reflns_number_total             7840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0337_suppl.cif
_cod_data_source_block           mg5
_cod_database_code               8105478
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.872
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 P1A-F1A \\sim P1A-F2A \\sim P1A-F3A \\sim P1A-F6A \\sim P1A-F5A \\sim P1A-F4A
 with sigma of 0.02
 P1A-F1A \\sim P1B-F1B
 with sigma of 0.02
 F2A-F5A \\sim F4B-F3B
 with sigma of 0.04
 P1A-F5A \\sim P1B-F3B
 with sigma of 0.02
 F6A-F4A \\sim F2B-F5B
 with sigma of 0.04
 F2A-F6A \\sim F4B-F2B
 with sigma of 0.04
 F2A-F4A \\sim F4B-F5B
 with sigma of 0.04
 P1A-F2A \\sim P1B-F4B
 with sigma of 0.04
 P1A-F6A \\sim P1B-F2B
 with sigma of 0.04
 P1A-F4A \\sim P1B-F5B
 with sigma of 0.04
 F6A-F5A \\sim F2B-F3B
 with sigma of 0.04
 F1A-F2A \\sim F1B-F4B
 with sigma of 0.04
 F5A-F4A \\sim F3B-F5B
 with sigma of 0.04
 F1A-F6A \\sim F1B-F2B
 with sigma of 0.04
 F1A-F5A \\sim F1B-F3B
 with sigma of 0.04
 F1A-F4A \\sim F1B-F5B
 with sigma of 0.04
 P1A-F3A \\sim P1A-F1A \\sim P1A-F5A \\sim P1A-F4A \\sim P1A-F2A \\sim P1A-F6A
 with sigma of 0.02
 F1B-F5B \\sim F1B-F3B \\sim F1B-F6B \\sim F1B-F2B \\sim F5B-F4B \\sim F5B-F6B
\\sim F5B-F2B \\sim F3B-F4B
 \\sim F3B-F2B \\sim F4B-F6B \\sim F4B-F2B
 with sigma of 0.04
 P1B-F1B \\sim P1B-F5B \\sim P1B-F3B \\sim P1B-F4B \\sim P1B-F6B \\sim P1B-F2B
 with sigma of 0.02
 F3C-F6C \\sim F3C-F2C \\sim F3C-F4C \\sim F6C-F2C \\sim F6C-F5C \\sim F6C-F4C
\\sim F2C-F5C \\sim F2C-F1C
 \\sim F5C-F4C \\sim F5C-F1C
 with sigma of 0.04
 F3A-F1A \\sim F3A-F5A \\sim F3A-F4A \\sim F3A-F2A \\sim F1A-F5A \\sim F1A-F4A
\\sim F1A-F6A \\sim F5A-F2A
 \\sim F5A-F6A \\sim F4A-F2A \\sim F4A-F6A \\sim F2A-F6A
 with sigma of 0.04
 P1C-F3C \\sim P1C-F6C \\sim P1C-F2C \\sim P1C-F5C \\sim P1C-F4C \\sim P1C-F1C
 with sigma of 0.02
3. Rigid bond restraints
 P1A, F1A, F2A, F3A, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
P1A \\sim F1A \\sim F2A \\sim F3A \\sim F4A \\sim F5A \\sim F6A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(F4B) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F1B) \\sim Ueq, Uanis(P1B) \\sim Ueq, Uanis(F5B) \\sim Ueq, Uanis(F2B)
\\sim Ueq, Uanis(F3B) \\sim Ueq, Uanis(F4B) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(P1A) \\sim Ueq, Uanis(F6A) \\sim Ueq, Uanis(F4A) \\sim Ueq, Uanis(F1A)
\\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F2A) \\sim Ueq, Uanis(F3A) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(P1C) \\sim Ueq, Uanis(F2C) \\sim Ueq, Uanis(F5C) \\sim Ueq, Uanis(F4C)
\\sim Ueq, Uanis(F6C) \\sim Ueq, Uanis(F3C) \\sim Ueq, Uanis(F1C) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(P1B) \\sim Ueq, Uanis(F3B) \\sim Ueq, Uanis(F6B) \\sim Ueq, Uanis(F1B)
\\sim Ueq, Uanis(F5B) \\sim Ueq, Uanis(F4B) \\sim Ueq, Uanis(F2B) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F5C) = Uanis(F3C) = Uanis(F6C) = Uanis(F2C) = Uanis(F4C) = Uanis(F1C) =
Uanis(F6B) = Uanis(F4B) = Uanis(F2B) = Uanis(F5B) = Uanis(F3B) = Uanis(F1B)
5. Rigid body (RIGU) restrains
 P1A, F1A, F2A, F3A, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1B, F1B, F2B, F3B, F4B, F5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: P1A(0.4) F1A(0.4) F2A(0.4) F3A(0.4) F4A(0.4) F5A(0.4) F6A(0.4)
 P1B(0.3) F1B(0.3) F2B(0.3) F3B(0.3) F4B(0.3) F5B(0.3) F6B(0.3) P1C(0.3)
 F1C(0.3) F2C(0.3) F3C(0.3) F4C(0.3) F5C(0.3) F6C(0.3)
7.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C9(H9), C12(H12), C13(H13), C15(H15),
 C16(H16), C18(H18), C19(H19), C20(H20), C21(H21)
7.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C)
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