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_7703684
_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         'C27 H55 B2 N O2 P2, C3 H7'
_chemical_formula_sum            'C30 H62 B2 N O2 P2'
_chemical_formula_weight         552.36
_chemical_melting_point          ?
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 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                 102.897(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.6216(4)
_cell_length_b                   7.71400(10)
_cell_length_c                   35.6578(6)
_cell_measurement_reflns_used    6140
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.3620
_cell_measurement_theta_min      3.4710
_cell_volume                     6869.80(19)
_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    -67.00  35.00   1.00    5.50    --  -41.02  37.00  90.00  102
  2  \w    -92.00  -2.00   1.00    5.50    --  -41.02 125.00-180.00   90
  3  \w   -115.00 -11.00   1.00    5.50    --  -41.02 -57.00 -60.00  104
  4  \w    100.00 178.00   1.00   22.00    --  108.00 111.00  30.00   78
  5  \w    100.00 178.00   1.00   22.00    --  108.00 111.00-180.00   78
  6  \w    100.00 178.00   1.00   22.00    --  108.00 114.00 113.00   78
  7  \w     34.00 138.00   1.00   22.00    --  108.00 -61.00  30.00  104
  8  \w     78.00 178.00   1.00   22.00    --  108.00  61.00   0.00  100
  9  \w     80.00 178.00   1.00   22.00    --  108.00  45.00 -60.00   98
 10  \w     34.00 138.00   1.00   22.00    --  108.00 -61.00-150.00  104
 11  \w     30.00 113.00   1.00   22.00    --  108.00-111.00  60.00   83
 12  \w   -115.00 -11.00   1.00    5.50    --  -41.02 -57.00-180.00  104
 13  \w   -120.00 -80.00   1.00    5.50    --  -41.02 -77.00  30.00   40
 14  \w   -115.00 -11.00   1.00    5.50    --  -41.02 -57.00  90.00  104
;
_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      -0.0509041000
_diffrn_orient_matrix_UB_12      -0.0162633000
_diffrn_orient_matrix_UB_13      0.0159681000
_diffrn_orient_matrix_UB_21      0.0328637000
_diffrn_orient_matrix_UB_22      0.0426083000
_diffrn_orient_matrix_UB_23      0.0406553000
_diffrn_orient_matrix_UB_31      -0.0114636000
_diffrn_orient_matrix_UB_32      0.1944546000
_diffrn_orient_matrix_UB_33      -0.0075693000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0708
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            11065
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        70.073
_diffrn_reflns_theta_max         70.073
_diffrn_reflns_theta_min         6.367
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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    1.068
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2440
_exptl_crystal_recrystallization_method 'Crystals grown from hexane at 278 K'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.917
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         11065
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      0.917
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0448
_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^)+(0.0712P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8318
_reflns_number_total             11065
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9913\% 
 around [0.96 0.00 -0.30] (reciprocal) or [1.00 0.00 -0.00] (direct)
;
_cod_data_source_file            c9dt04474d3.cif
_cod_data_source_block           0507abc19s
_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_original_cell_volume        6869.79(19)
_cod_database_code               7703684
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6692(8)
 0.3308(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All B(H,H,H) groups, All C(H,H,H) groups
3. Restrained distances
 C91-C92B \\sim C92A-C91
 with sigma of 0.01
 C92A_$1-C92A \\sim C92B_$1-C92B
 with sigma of 0.01
 B2-H2A \\sim B2-H2B \\sim B2-H2C \\sim B3-H3C \\sim B3-H3A \\sim B3-H3B
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C92B) = Uanis(C92A)
5. Others
 Sof(H91C)=Sof(H91D)=Sof(C92B)=Sof(H92C)=Sof(H92D)=1-FVAR(1)
 Sof(H91A)=Sof(H91B)=Sof(C92A)=Sof(H92A)=Sof(H92B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 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), C91(H91A,H91B), C91(H91C,H91D), C92A(H92A,H92B), C92B(H92C,H92D)
6.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105)
6.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), C90(H90A,H90B,H90C)
6.d Idealised Me refined as rotating group with stretchable bonds:
 B2(H2A,H2B,H2C), B3(H3A,H3B,H3C)
;
_shelx_res_checksum              30556
_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 3.432
_oxdiff_exptl_absorpt_empirical_full_min 0.463
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2