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_7701770
_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         'C38 H72 B10 Ni2 O4 P4 S2'
_chemical_formula_sum            'C38 H72 B10 Ni2 O4 P4 S2'
_chemical_formula_weight         1006.47
_chemical_name_systematic        'di Ni POCOP iPr CB'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_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            4
_cell_length_a                   18.7762(6)
_cell_length_b                   15.5899(5)
_cell_length_c                   17.6800(6)
_cell_measurement_reflns_used    7618
_cell_measurement_temperature    295.16(10)
_cell_measurement_theta_max      24.7620
_cell_measurement_theta_min      3.6620
_cell_volume                     5175.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.42a (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      295.16
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_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    -50.00   3.00   1.00   14.75    --  -11.77  92.00  65.00   53
  2  \w    -17.00  54.00   1.00   14.75    --  -11.77  50.00 -40.00   71
  3  \w     37.00  72.00   1.00   14.75    --   10.83-178.00 -60.00   35
  4  \w    -20.00  29.00   1.00   14.75    --  -11.77 -99.00 150.00   49
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24457
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.425
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.42a (Rigaku Oxford Diffraction, 2019)
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    1.292
_exptl_crystal_description       block
_exptl_crystal_F_000             2120
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         5072
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+6.3057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1318
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3745
_reflns_number_total             5072
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02825k2.cif
_cod_data_source_block           cbl-20180409-ni
_cod_database_code               7701770
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.670
_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. Restrained distances
 C8B-C7B
 1.6 with sigma of 0.001
 C7B-P1
 1.8 with sigma of 0.001
 C9A-C7A \\sim C9B-C7B \\sim C8A-C7A \\sim C8B-C7B
 with sigma of 0.001
 C11-C10 \\sim C12A-C10A \\sim C12-C10 \\sim C11A-C10A
 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(C11A) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C10A)
\\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 S1, B5, B2, C19, B4, B1, B3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 S1A, B5A, B2A, C19A, B4A, B1A, B3A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(S1A)=Sof(C19A)=Sof(B1A)=Sof(H1A)=Sof(B3A)=Sof(H3AA)=Sof(B2A)=Sof(H2A)=
 Sof(B5A)=Sof(H5AA)=Sof(B4A)=Sof(H4AA)=Sof(C7A)=Sof(H7A)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(H9AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C10A)=Sof(H10A)=
 Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C11A)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=1-FVAR(1)
 Sof(S1)=Sof(C19)=Sof(B1)=Sof(H1)=Sof(C10)=Sof(H10)=Sof(B3)=Sof(H3A)=Sof(B2)=
 Sof(H2)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=Sof(B5)=Sof(H5A)=Sof(C11)=
 Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(H9BC)=Sof(C7B)=
 Sof(H7B)=Sof(C8B)=Sof(H8BA)=Sof(H8BB)=Sof(H8BC)=Sof(B4)=Sof(H4A)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C13(H13), C16(H16), C10(H10), C7B(H7B), C7A(H7A), C10A(H10A)
6.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C3(H3)
6.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C17(H17A,H17B,
 H17C), C12(H12A,H12B,H12C), C11(H11A,H11B,H11C), C9B(H9BA,H9BB,H9BC), C8B(H8BA,
 H8BB,H8BC), C9A(H9AA,H9AB,H9AC), C8A(H8AA,H8AB,H8AC), C12A(H12D,H12E,H12F),
 C11A(H11D,H11E,H11F)
6.d Boron cage BH refined with riding coordinates:
 B1(H1), B3(H3A), B2(H2), B5(H5A), B4(H4A), B1A(H1A), B3A(H3AA), B2A(H2A),
 B5A(H5AA), B4A(H4AA)
;
_shelx_res_checksum              67869
_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
;