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_7701766
_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         'C24 H36 Ni O2 P2'
_chemical_formula_sum            'C24 H36 Ni O2 P2'
_chemical_formula_weight         477.18
_chemical_name_systematic        iPr-POCOP-Ni-Ph
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-18
_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                 112.390(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.34150(10)
_cell_length_b                   16.5817(3)
_cell_length_c                   9.28950(10)
_cell_measurement_reflns_used    7034
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      72.4540
_cell_measurement_theta_min      5.0850
_cell_volume                     1188.02(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      170.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.978
_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   -109.00 -14.00   1.00    1.00    --  -40.52 149.00-155.00   95
  2  \w   -114.00 -58.00   1.00    1.00    --  -40.52-149.00 158.00   56
  3  \w    -90.00   0.00   1.00    1.00    --  -40.52 123.00  41.00   90
  4  \w     36.00 112.00   1.00    1.00    --   40.52-149.00 158.00   76
  5  \w     95.00 177.00   1.00    1.00    --  103.55 123.00  41.00   82
  6  \w     36.00 134.00   1.00    1.00    --  103.55-149.00 158.00   98
  7  \w     30.00 116.00   1.00    1.00    --  103.55-123.00 -38.00   86
  8  \w     79.00 173.00   1.00    1.00    --  103.55 149.00-155.00   94
  9  \w    -69.00  33.00   1.00    1.00    --  -40.52  57.00-180.00  102
 10  \w   -113.00 -12.00   1.00    1.00    --  -40.52 -57.00  30.00  101
 11  \w     27.00 112.00   1.00    1.00    --  103.55-111.00-180.00   85
 12  \w     78.00 177.00   1.00    1.00    --  103.55  45.00-150.00   99
 13  \w    100.00 178.00   1.00    1.00    --  103.55 111.00  90.00   78
 14  \w     71.00 178.00   1.00    1.00    --  103.55  77.00  60.00  107
 15  \w     31.00 129.00   1.00    1.00    --  103.55 -45.00  90.00   98
 16  \w   -113.00 -77.00   1.00    1.00    --  -40.52 -57.00 -90.00   36
 17  \w   -117.00  -8.00   1.00    1.00    --  -40.52 -77.00-180.00  109
;
_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      -0.0204384000
_diffrn_orient_matrix_UB_12      0.0924122000
_diffrn_orient_matrix_UB_13      -0.0071566000
_diffrn_orient_matrix_UB_21      0.0534956000
_diffrn_orient_matrix_UB_22      0.0025055000
_diffrn_orient_matrix_UB_23      -0.1414777000
_diffrn_orient_matrix_UB_31      -0.1913268000
_diffrn_orient_matrix_UB_32      -0.0092070000
_diffrn_orient_matrix_UB_33      -0.1099944000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9944
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.363
_diffrn_reflns_theta_min         5.149
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.577
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26470
_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    1.334
_exptl_crystal_description       plate
_exptl_crystal_F_000             508
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.912
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0664P)^2^+0.5543P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1037
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2290
_reflns_number_total             2379
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02825k2.cif
_cod_data_source_block           cbl-niph
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               7701766
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Ni1 P1 C1 O1 H1'
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.783
_diffrn_oxdiff_digest_frames
;
0119be45fd796cb5e3199507fc6869987d00029759e
;
_diffrn_oxdiff_digest_hkl
;
01e44ef84816ebf8396f7e9d5afa2913e5999c
;
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C5(H5), C8(H8)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C12(H12), C16(H16), C4(H4), C3(H3), C15(H15), C14(H14)
2.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              17394
_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 3.922
_oxdiff_exptl_absorpt_empirical_full_min 0.492