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_7701769
_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         'C16 H48 B20 Ni P2 S2'
_chemical_formula_sum            'C16 H48 B20 Ni P2 S2'
_chemical_formula_weight         641.51
_chemical_name_systematic        NISP
_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   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-05 deposited with the CCDC.	2019-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.711(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.4737(2)
_cell_length_b                   9.9192(2)
_cell_length_c                   14.6100(3)
_cell_measurement_reflns_used    4583
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.5950
_cell_measurement_theta_min      3.9040
_cell_volume                     1633.79(6)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_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    -71.00  32.00   1.00    1.43    --  -40.77  66.00 107.00  103
  2  \w   -114.00 -11.00   1.00    1.43    --  -40.77 -66.00 -27.00  103
  3  \w     31.00 134.00   1.00    5.72    --  103.86 -66.00 -27.00  103
  4  \w     74.00 177.00   1.00    5.72    --  103.86  66.00 107.00  103
  5  \w      1.00  82.00   1.00    1.43    --   40.77 -99.00-180.00   81
  6  \w     23.00  97.00   1.00    1.43    --   40.77-125.00-120.00   74
  7  \w     21.00 110.00   1.00    5.72    --  103.86 -94.00  30.00   89
  8  \w     32.00 133.00   1.00    5.72    --  103.86 -61.00-150.00  101
  9  \w     32.00 108.00   1.00    5.72    --  103.86-125.00-180.00   76
 10  \w     79.00 169.00   1.00    5.72    --  103.86  45.00-180.00   90
 11  \w    125.00 151.00   1.00    5.72    --  103.86 125.00 -30.00   26
 12  \w     42.00 108.00   1.00    5.72    --  103.86 -94.00-180.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1021154000
_diffrn_orient_matrix_UB_12      0.0902970000
_diffrn_orient_matrix_UB_13      -0.0487572000
_diffrn_orient_matrix_UB_21      0.0868011000
_diffrn_orient_matrix_UB_22      0.0752872000
_diffrn_orient_matrix_UB_23      -0.0508230000
_diffrn_orient_matrix_UB_31      -0.0264844000
_diffrn_orient_matrix_UB_32      -0.1015117000
_diffrn_orient_matrix_UB_33      -0.0809698000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9910
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.701
_diffrn_reflns_theta_min         3.921
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.031
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88801
_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    1.304
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3179
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+0.4654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0659
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2804
_reflns_number_total             3179
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02825k2.cif
_cod_data_source_block           cbl-20190320
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7701769
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Ni1 O1 H1 C1 P1 B1 S1'
_shelx_estimated_absorpt_t_max   0.377
_shelx_estimated_absorpt_t_min   0.264
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
;
_shelx_res_checksum              45126
_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 1.246
_oxdiff_exptl_absorpt_empirical_full_min 0.827