#------------------------------------------------------------------------------
#$Date: 2019-11-05 19:51:01 +0200 (Tue, 05 Nov 2019) $
#$Revision: 223354 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/17/7701766.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7701766
loop_
_publ_author_name
'Cao, Bula'
'Ding, Yazhou'
'Fang, Fei'
'Chang, Jiarui'
'Zhang, Jie'
'Li, Shujun'
'Chen, Xuenian'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -109.00 -14.00   1.00    1.00    --  -40.52 149.00-155.00   95
  2  ω   -114.00 -58.00   1.00    1.00    --  -40.52-149.00 158.00   56
  3  ω    -90.00   0.00   1.00    1.00    --  -40.52 123.00  41.00   90
  4  ω     36.00 112.00   1.00    1.00    --   40.52-149.00 158.00   76
  5  ω     95.00 177.00   1.00    1.00    --  103.55 123.00  41.00   82
  6  ω     36.00 134.00   1.00    1.00    --  103.55-149.00 158.00   98
  7  ω     30.00 116.00   1.00    1.00    --  103.55-123.00 -38.00   86
  8  ω     79.00 173.00   1.00    1.00    --  103.55 149.00-155.00   94
  9  ω    -69.00  33.00   1.00    1.00    --  -40.52  57.00-180.00  102
 10  ω   -113.00 -12.00   1.00    1.00    --  -40.52 -57.00  30.00  101
 11  ω     27.00 112.00   1.00    1.00    --  103.55-111.00-180.00   85
 12  ω     78.00 177.00   1.00    1.00    --  103.55  45.00-150.00   99
 13  ω    100.00 178.00   1.00    1.00    --  103.55 111.00  90.00   78
 14  ω     71.00 178.00   1.00    1.00    --  103.55  77.00  60.00  107
 15  ω     31.00 129.00   1.00    1.00    --  103.55 -45.00  90.00   98
 16  ω   -113.00 -77.00   1.00    1.00    --  -40.52 -57.00 -90.00   36
 17  ω   -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       'ω 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/[σ²(Fo²)+(0.0664P)²+0.5543P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ni1 Ni 0.48454(5) 0.750000 0.75331(4) 0.01312(15) Uani 1 2 d S T P
P1 P 0.47068(5) 0.62269(2) 0.77811(5) 0.01563(15) Uani 1 1 d . . .
O1 O 0.35296(16) 0.60650(7) 0.88550(14) 0.0212(3) Uani 1 1 d . . .
C11 C 0.6131(3) 0.750000 0.6172(3) 0.0159(5) Uani 1 2 d S T P
C2 C 0.3054(2) 0.67867(10) 0.93515(19) 0.0173(4) Uani 1 1 d . . .
C13 C 0.8853(3) 0.750000 0.5755(3) 0.0228(5) Uani 1 2 d S T P
H13 H 1.005858 0.750000 0.617354 0.027 Uiso 1 2 calc RS T P
C12 C 0.7949(3) 0.750000 0.6737(3) 0.0192(5) Uani 1 2 d S T P
H12 H 0.857005 0.750000 0.780806 0.023 Uiso 1 2 calc RS T P
C16 C 0.5281(3) 0.750000 0.4547(3) 0.0199(5) Uani 1 2 d S T P
H16 H 0.407512 0.750000 0.411936 0.024 Uiso 1 2 calc RS T P
C4 C 0.1690(3) 0.750000 1.0797(3) 0.0205(5) Uani 1 2 d S T P
H4 H 0.107944 0.749999 1.145156 0.025 Uiso 1 2 calc RS T P
C3 C 0.2136(2) 0.67667(11) 1.0319(2) 0.0199(4) Uani 1 1 d . . .
H3 H 0.182720 0.627962 1.063793 0.024 Uiso 1 1 calc R . .
C5 C 0.6692(2) 0.56890(11) 0.89549(19) 0.0207(4) Uani 1 1 d . . .
H5 H 0.636447 0.519176 0.934396 0.025 Uiso 1 1 calc R . .
C1 C 0.3544(3) 0.750000 0.8838(3) 0.0153(5) Uani 1 2 d S T P
C15 C 0.6172(3) 0.750000 0.3553(3) 0.0229(5) Uani 1 2 d S T P
H15 H 0.556002 0.750000 0.248134 0.028 Uiso 1 2 calc RS T P
C14 C 0.7964(3) 0.750000 0.4148(3) 0.0225(5) Uani 1 2 d S T P
H14 H 0.856528 0.750000 0.348610 0.027 Uiso 1 2 calc RS T P
C8 C 0.3566(2) 0.56029(11) 0.6074(2) 0.0215(4) Uani 1 1 d . . .
H8 H 0.425444 0.560293 0.542280 0.026 Uiso 1 1 calc R . .
C6 C 0.7720(3) 0.62200(13) 1.0358(2) 0.0287(4) Uani 1 1 d . . .
H6A H 0.810681 0.669779 1.000275 0.043 Uiso 1 1 calc GR . .
H6B H 0.870582 0.592598 1.104585 0.043 Uiso 1 1 calc GR . .
H6C H 0.699083 0.636835 1.090309 0.043 Uiso 1 1 calc GR . .
C7 C 0.7782(2) 0.54611(12) 0.8012(2) 0.0273(4) Uani 1 1 d . . .
H7A H 0.715081 0.508427 0.721196 0.041 Uiso 1 1 calc GR . .
H7B H 0.884928 0.521944 0.868796 0.041 Uiso 1 1 calc GR . .
H7C H 0.802954 0.593659 0.754387 0.041 Uiso 1 1 calc GR . .
C9 C 0.1818(2) 0.59970(13) 0.5133(2) 0.0321(5) Uani 1 1 d . . .
H9A H 0.112433 0.601848 0.575283 0.048 Uiso 1 1 calc GR . .
H9B H 0.122674 0.568536 0.421081 0.048 Uiso 1 1 calc GR . .
H9C H 0.200630 0.653398 0.484413 0.048 Uiso 1 1 calc GR . .
C10 C 0.3339(3) 0.47259(12) 0.6465(2) 0.0337(5) Uani 1 1 d . . .
H10A H 0.445486 0.449113 0.702958 0.051 Uiso 1 1 calc GR . .
H10B H 0.276587 0.442951 0.551947 0.051 Uiso 1 1 calc GR . .
H10C H 0.265213 0.470613 0.709153 0.051 Uiso 1 1 calc GR . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
P1 Ni1 P1 164.12(3) . 4_575
C11 Ni1 P1 97.835(15) . 4_575
C11 Ni1 P1 97.835(15) . .
C1 Ni1 P1 82.189(16) . .
C1 Ni1 P1 82.190(15) . 4_575
C1 Ni1 C11 178.97(9) . .
O1 P1 Ni1 107.02(5) . .
O1 P1 C5 99.82(7) . .
O1 P1 C8 101.39(7) . .
C5 P1 Ni1 118.22(6) . .
C8 P1 Ni1 119.91(6) . .
C8 P1 C5 107.14(8) . .
C2 O1 P1 111.52(10) . .
C12 C11 Ni1 122.81(17) . .
C16 C11 Ni1 121.46(18) . .
C16 C11 C12 115.7(2) . .
O1 C2 C1 117.26(15) . .
C3 C2 O1 119.45(15) . .
C3 C2 C1 123.29(16) . .
C12 C13 H13 119.8 . .
C12 C13 C14 120.3(2) . .
C14 C13 H13 119.8 . .
C11 C12 H12 118.8 . .
C13 C12 C11 122.3(2) . .
C13 C12 H12 118.8 . .
C11 C16 H16 118.8 . .
C15 C16 C11 122.5(2) . .
C15 C16 H16 118.8 . .
C3 C4 H4 119.2 . .
C3 C4 H4 119.2 4_575 .
C3 C4 C3 121.6(2) . 4_575
C2 C3 C4 117.83(16) . .
C2 C3 H3 121.1 . .
C4 C3 H3 121.1 . .
P1 C5 H5 108.3 . .
C6 C5 P1 108.19(12) . .
C6 C5 H5 108.3 . .
C7 C5 P1 112.28(12) . .
C7 C5 H5 108.3 . .
C7 C5 C6 111.47(15) . .
C2 C1 Ni1 121.92(10) . .
C2 C1 Ni1 121.92(11) 4_575 .
C2 C1 C2 116.2(2) 4_575 .
C16 C15 H15 119.8 . .
C14 C15 C16 120.4(2) . .
C14 C15 H15 119.8 . .
C13 C14 H14 120.6 . .
C15 C14 C13 118.8(2) . .
C15 C14 H14 120.6 . .
P1 C8 H8 107.6 . .
C9 C8 P1 108.76(13) . .
C9 C8 H8 107.6 . .
C10 C8 P1 113.78(13) . .
C10 C8 H8 107.6 . .
C10 C8 C9 111.36(16) . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6B 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7B 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9B 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10B 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 P1 2.1315(4) 4_575
Ni1 P1 2.1315(4) .
Ni1 C11 1.944(2) .
Ni1 C1 1.911(2) .
P1 O1 1.6666(12) .
P1 C5 1.8308(17) .
P1 C8 1.8278(18) .
O1 C2 1.393(2) .
C11 C12 1.403(3) .
C11 C16 1.402(3) .
C2 C3 1.385(2) .
C2 C1 1.394(2) .
C13 H13 0.9300 .
C13 C12 1.387(3) .
C13 C14 1.391(3) .
C12 H12 0.9300 .
C16 H16 0.9300 .
C16 C15 1.389(3) .
C4 H4 0.9300 .
C4 C3 1.393(2) 4_575
C4 C3 1.393(2) .
C3 H3 0.9300 .
C5 H5 0.9800 .
C5 C6 1.536(3) .
C5 C7 1.531(2) .
C15 H15 0.9300 .
C15 C14 1.382(4) .
C14 H14 0.9300 .
C8 H8 0.9800 .
C8 C9 1.532(3) .
C8 C10 1.528(3) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
