Synthesis and rhodium complexes of macrocyclic PNP and PONOP pincer ligands.
Hood, Thomas M.; Gyton, Matthew R.; Chaplin, Adrian B.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 2077–2086; doi:10.1039/c9dt04474d

data_7703687
_publ_section_title
;
 Synthesis and rhodium complexes of macrocyclic PNP and PONOP pincer
 ligands.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2077
_journal_page_last               2086
_journal_paper_doi               10.1039/c9dt04474d
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C41 H61 N P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C73 H73 B F24 N P2 Rh'
_chemical_formula_weight         1595.98
_chemical_melting_point          ?
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-05-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-11-20 deposited with the CCDC.	2019-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3071(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.62740(16)
_cell_length_b                   13.36471(14)
_cell_length_c                   39.2179(5)
_cell_measurement_reflns_used    51707
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.3450
_cell_measurement_theta_min      2.7230
_cell_volume                     7111.99(14)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6093
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -110.00 -56.00   0.30    4.00    --  -23.16 178.00-180.00  180
  2  \w     -8.00 100.00   0.30    4.00    --   24.25  77.00   0.00  360
  3  \w    -48.00  51.00   0.30    4.00    --   24.25 -57.00-150.00  330
  4  \w    -50.00  49.00   0.30    4.00    --   24.25 -37.00 -60.00  330
  5  \w    -47.00  50.20   0.30    4.00    --  -23.16  37.00 120.00  324
  6  \w    -95.00 -69.80   0.30    4.00    --  -23.16 -57.00-150.00   84
  7  \w     -8.00 100.00   0.30    4.00    --   24.25  77.00 150.00  360
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'Rigaku Oxford Diffraction: SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0238650000
_diffrn_orient_matrix_UB_12      0.0389720000
_diffrn_orient_matrix_UB_13      -0.0098498000
_diffrn_orient_matrix_UB_21      -0.0046097000
_diffrn_orient_matrix_UB_22      -0.0317926000
_diffrn_orient_matrix_UB_23      -0.0145453000
_diffrn_orient_matrix_UB_31      -0.0462789000
_diffrn_orient_matrix_UB_32      -0.0169287000
_diffrn_orient_matrix_UB_33      0.0046279000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0277
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            113645
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        29.575
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         3.002
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3256
_exptl_crystal_recrystallization_method
'Crystals grown from CH2Cl2-pentane at 293 K'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.599
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     944
_refine_ls_number_reflns         19935
_refine_ls_number_restraints     342
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0360
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+6.5345P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0864
_refine_ls_wR_factor_ref         0.0901
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17587
_reflns_number_total             19935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04474d3.cif
_cod_data_source_block           0410abc18s
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7703687
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 C216-F10 \\sim C216-F11 \\sim C216-F12 \\sim C216-F10A \\sim C216-F11A \\sim
C216-F12A
 with sigma of 0.01
 F10-F11 \\sim F11-F12 \\sim F12-F10 \\sim F10A-F11A \\sim F11A-F12A \\sim
F12A-F10A
 with sigma of 0.01
 C213-F10 \\sim C213-F11 \\sim C213-F12 \\sim C213-F10A \\sim C213-F11A \\sim
C213-F12A
 with sigma of 0.01
 C232-F22 \\sim C232-F23 \\sim C232-F24 \\sim C232-F22A \\sim C232-F23A \\sim
C232-F24A
 with sigma of 0.01
 F22-F23 \\sim F23-F24 \\sim F24-F22 \\sim F22A-F23A \\sim F23A-F24A \\sim
F24A-F22A
 with sigma of 0.01
 C229-F22 \\sim C229-F23 \\sim C229-F24 \\sim C229-F22A \\sim C229-F23A \\sim
C229-F24A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F5 \\sim F6 \\sim F7 \\sim F8 \\sim F9
\\sim F10 \\sim F10A \\sim F11 \\sim F11A \\sim F12 \\sim F12A \\sim F13 \\sim
F14 \\sim F15 \\sim F16 \\sim F17 \\sim F18 \\sim F19 \\sim F20 \\sim F21 \\sim
F22 \\sim F22A \\sim F23 \\sim F23A \\sim F24 \\sim F24A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F5) \\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F8)
\\sim Ueq, Uanis(F9) \\sim Ueq, Uanis(F10) \\sim Ueq, Uanis(F10A) \\sim Ueq,
Uanis(F11) \\sim Ueq, Uanis(F11A) \\sim Ueq, Uanis(F12) \\sim Ueq, Uanis(F12A)
\\sim Ueq, Uanis(F13) \\sim Ueq, Uanis(F14) \\sim Ueq, Uanis(F15) \\sim Ueq,
Uanis(F16) \\sim Ueq, Uanis(F17) \\sim Ueq, Uanis(F18) \\sim Ueq, Uanis(F19)
\\sim Ueq, Uanis(F20) \\sim Ueq, Uanis(F21) \\sim Ueq, Uanis(F22) \\sim Ueq,
Uanis(F22A) \\sim Ueq, Uanis(F23) \\sim Ueq, Uanis(F23A) \\sim Ueq, Uanis(F24)
\\sim Ueq, Uanis(F24A) \\sim Ueq: with sigma of 0.007 and sigma for terminal
atoms of 0.014
Uanis(F22) = Uanis(F22A)
Uanis(F24) = Uanis(F24A)
Uanis(F23) = Uanis(F23A)
Uanis(F10A) = Uanis(F10)
Uanis(F11A) = Uanis(F11)
Uanis(F12) = Uanis(F12A)
4. Others
 Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(1)
 Sof(F22)=Sof(F23)=Sof(F24)=FVAR(1)
 Fixed Sof: F10(0.5) F10A(0.5) F11(0.5) F11A(0.5) F12(0.5) F12A(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C107(H10C,H10D), C108(H10A,H10B), C117(H11A,H11B), C118(H11W,H11X), C119(H11I,
 H11J), C120(H12K,H12L), C121(H12C,H12D), C122(H12M,H12N), C123(H12G,H12H),
 C124(H12O,H12P), C125(H12A,H12B), C126(H12Q,H12R), C127(H12I,H12J), C128(H12S,
 H12T), C129(H12E,H12F), C130(H13A,H13B)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C11(H11), C12(H12), C13(H13), C14(H14),
 C103(H103), C104(H104), C105(H105), C202(H202), C204(H204), C206(H206),
 C210(H210), C212(H212), C214(H214), C218(H218), C220(H220), C222(H222),
 C226(H226), C228(H228), C230(H230)
5.c Idealised Me refined as rotating group:
 C110(H11K,H11L,H11M), C111(H11C,H11D,H11E), C112(H11N,H11O,H11P), C114(H11Q,
 H11R,H11S), C115(H11F,H11G,H11H), C116(H11T,H11U,H11V)
;
_shelx_res_checksum              81147
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.339
_oxdiff_exptl_absorpt_empirical_full_min 0.791