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_7703683
_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         'C29 H59 B2 N P2'
_chemical_formula_sum            'C29 H59 B2 N P2'
_chemical_formula_weight         505.33
_chemical_melting_point          ?
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-11-07
_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                 114.2091(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.36586(11)
_cell_length_b                   26.05266(18)
_cell_length_c                   11.08994(10)
_cell_measurement_reflns_used    24678
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.4420
_cell_measurement_theta_min      3.3350
_cell_volume                     3258.57(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_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_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_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   -117.00 -18.00   1.00    3.50    --  -42.07 -37.00 -30.00   99
  2  \w    -66.00  32.00   1.00    3.50    --  -42.07  37.00 -30.00   98
  3  \w     23.00  98.00   1.00    3.50    --   42.07-125.00 -90.00   75
  4  \w     35.00 136.00   1.00   14.00    --  107.00 -61.00  90.00  101
  5  \w     78.00 178.00   1.00   14.00    --  107.00  61.00 -30.00  100
  6  \w     24.00 110.00   1.00   14.00    --  107.00 -94.00 -30.00   86
  7  \w     94.00 178.00   1.00   14.00    --  107.00 125.00-180.00   84
  8  \w     81.00 178.00   1.00   14.00    --  107.00  45.00 -90.00   97
  9  \w     34.00 118.00   1.00   14.00    --  107.00-125.00-180.00   84
 10  \w     74.00 178.00   1.00   14.00    --  107.00  77.00   0.00  104
 11  \w     81.00 178.00   1.00   14.00    --  107.00  45.00-180.00   97
 12  \w     34.00 118.00   1.00   14.00    --  107.00-125.00  90.00   84
 13  \w     94.00 178.00   1.00   14.00    --  107.00 125.00-150.00   84
 14  \w     35.00 136.00   1.00   14.00    --  107.00 -61.00 -30.00  101
 15  \w   -114.00 -14.00   1.00    3.50    --  -42.07 -57.00 -90.00  100
 16  \w   -114.00 -14.00   1.00    3.50    --  -42.07 -57.00-180.00  100
 17  \w   -114.00 -14.00   1.00    3.50    --  -42.07 -57.00  90.00  100
 18  \w     78.00 178.00   1.00   14.00    --  107.00  61.00 120.00  100
 19  \w     78.00 178.00   1.00   14.00    --  107.00  61.00-120.00  100
 20  \w     78.00 178.00   1.00   14.00    --  107.00  61.00-150.00  100
 21  \w     94.00 178.00   1.00   14.00    --  107.00 125.00  30.00   84
 22  \w     78.00 178.00   1.00   14.00    --  107.00  61.00 -60.00  100
 23  \w     78.00 178.00   1.00   14.00    --  107.00  61.00 150.00  100
 24  \w     34.00 118.00   1.00   14.00    --  107.00-125.00 -90.00   84
 25  \w     74.00 178.00   1.00   14.00    --  107.00  77.00  30.00  104
 26  \w     81.00 178.00   1.00   14.00    --  107.00  45.00  90.00   97
 27  \w   -118.00 -63.00   1.00    3.50    --  -42.07 -77.00  30.00   55
 28  \w      1.00  83.00   1.00    3.50    --   42.07 -99.00  60.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0298007000
_diffrn_orient_matrix_UB_12      -0.0166078000
_diffrn_orient_matrix_UB_13      -0.1161294000
_diffrn_orient_matrix_UB_21      0.1330528000
_diffrn_orient_matrix_UB_22      0.0073542000
_diffrn_orient_matrix_UB_23      0.0872837000
_diffrn_orient_matrix_UB_31      0.0085659000
_diffrn_orient_matrix_UB_32      -0.0562859000
_diffrn_orient_matrix_UB_33      0.0457205000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            51452
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        70.063
_diffrn_reflns_theta_max         70.063
_diffrn_reflns_theta_min         6.433
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.309
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.030
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_recrystallization_method 'Crystals grown from hexane at 278 K'
_exptl_crystal_size_max          0.467
_exptl_crystal_size_mid          0.278
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.794
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6186
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0515
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0689P)^2^+2.1991P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1304
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5591
_reflns_number_total             6186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04474d3.cif
_cod_data_source_block           0506abc19s
_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               7703683
_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 B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 B3-H3B \\sim B3-H3C \\sim B3-H3A \\sim B2-H2C \\sim B2-H2B \\sim B2-H2A
 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C107(H10A,H10B), C108(H10C,H10D), C117(H11S,H11T), C118(H11U,H11V), C119(H11W,
 H11X), C120(H12A,H12B), C121(H12C,H12D), C122(H12E,H12F), C123(H12G,H12H),
 C124(H12I,H12J), C125(H12K,H12L), C126(H12M,H12N), C127(H12O,H12P), C128(H12Q,
 H12R), C129(H12S,H12T), C130(H13A,H13B)
3.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105)
3.c Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C114(H11J,
 H11K,H11L), C115(H11M,H11N,H11O), C116(H11P,H11Q,H11R)
3.d Idealised Me refined as rotating group with stretchable bonds:
 B2(H2A,H2B,H2C), B3(H3A,H3B,H3C)
;
_shelx_res_checksum              11172
_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 5.597
_oxdiff_exptl_absorpt_empirical_full_min 0.536