The stability of group 10 metal POCOP pincer complexes: decomposition/reconstruction pathways of the pincer backbone.
Cao, Bula; Ding, Yazhou; Fang, Fei; Chang, Jiarui; Zhang, Jie; Li, Shujun; Chen, Xuenian; Dalton transactions (Cambridge, England : 2003) 48 (2019) 13760–13768; doi:10.1039/c9dt02825k

data_7701767
_publ_section_title
;
 The stability of group 10 metal POCOP pincer complexes:
 decomposition/reconstruction pathways of the pincer backbone.
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13760
_journal_page_last               13768
_journal_paper_doi               10.1039/c9dt02825k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C20 H42 B10 O2 P2 Pd'
_chemical_formula_sum            'C20 H42 B10 O2 P2 Pd'
_chemical_formula_weight         590.97
_chemical_name_systematic        iPr-POCOP-Pd-0-CB
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-02 deposited with the CCDC.	2019-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.2661(2)
_cell_length_b                   15.3835(2)
_cell_length_c                   28.9916(3)
_cell_measurement_reflns_used    8507
_cell_measurement_temperature    293.91(10)
_cell_measurement_theta_max      71.0740
_cell_measurement_theta_min      4.5610
_cell_volume                     5916.58(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.91(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0528
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.987
_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    -89.00  -2.00   1.00    1.00    --  -35.37 125.00 120.00   87
  2  \w   -103.00 -19.00   1.00    1.00    --  -35.37 -57.00   0.00   84
  3  \w     19.00 103.00   1.00    1.00    --   35.37  57.00-120.00   84
  4  \w    -32.00  52.00   1.00    1.00    --   35.37 -57.00 -60.00   84
  5  \w     85.00 176.00   1.00    2.78    --  106.50  30.00-180.00   91
  6  \w    100.00 176.00   1.00    2.78    --  106.50 111.00 120.00   76
  7  \w     37.00 109.00   1.00    2.78    --  106.50 -95.00  90.00   72
  8  \w     40.00 125.00   1.00    2.78    --  106.50 -61.00  30.00   85
  9  \w    100.00 176.00   1.00    2.78    --  106.50 111.00-180.00   76
 10  \w     88.00 173.00   1.00    2.78    --  106.50  61.00 -60.00   85
 11  \w    103.00 167.00   1.00    2.78    --  106.50 111.00  30.00   64
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0436331000
_diffrn_orient_matrix_UB_12      -0.0131612000
_diffrn_orient_matrix_UB_13      -0.0644971000
_diffrn_orient_matrix_UB_21      -0.0298171000
_diffrn_orient_matrix_UB_22      -0.0006933000
_diffrn_orient_matrix_UB_23      -0.0961478000
_diffrn_orient_matrix_UB_31      0.0055581000
_diffrn_orient_matrix_UB_32      0.0992607000
_diffrn_orient_matrix_UB_33      -0.0091759000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            11829
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.256
_diffrn_reflns_theta_min         4.658
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.194
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70040
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_description       block
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.620
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       0.00051(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2976
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0377
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0380P)^2^+15.8950P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2854
_reflns_number_total             2976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02825k2.cif
_cod_data_source_block           cbl-20181109
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               7701767
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'P1 C1 B1 H1 Pd1'
_shelx_estimated_absorpt_t_max   0.386
_shelx_estimated_absorpt_t_min   0.124
_reflns_odcompleteness_completeness 99.76
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All B(H) groups, All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(B4) \\sim Ueq, Uanis(B7) \\sim Ueq, Uanis(B2) \\sim Ueq, Uanis(B10) \\sim
Ueq, Uanis(B6) \\sim Ueq, Uanis(B3) \\sim Ueq, Uanis(B9) \\sim Ueq, Uanis(B8)
\\sim Ueq, Uanis(B5) \\sim Ueq, Uanis(B1) \\sim Ueq, Uanis(C12) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C2, B1, B2, B3, B4, B5, B6, C12, B7, B8, B9, B10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: B1(0.5) H1(0.5) B3(0.5) H3(0.5) B4(0.5) H4A(0.5) B5(0.5) H5A(0.5)
 B6(0.5) H6A(0.5) C12(0.5) H12(0.5) B7(0.5) H7A(0.5) B8(0.5) H8(0.5) B9(0.5)
 H9(0.5) B10(0.5) H10(0.5)
5.a Ternary CH refined with riding coordinates:
 C4(H4), C6(H6)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7)
5.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
5.d Boron cage BH refined with riding coordinates:
 B1(H1), B3(H3), B4(H4A), B5(H5A), B6(H6A), C12(H12), B7(H7A), B8(H8), B9(H9),
 B10(H10)
;
_shelx_res_checksum              22081
_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 1.390
_oxdiff_exptl_absorpt_empirical_full_min 0.671