Carbodiphosphorane-based nickel pincer complexes and their (de)protonated analogues: dimerisation, ligand tautomers and proton affinities.
Maser, Leon; Herritsch, Jan; Langer, Robert; Dalton transactions (Cambridge, England : 2003) 47 (2018) 10544–10552; doi:10.1039/c7dt04930g

data_7045647
_publ_section_title
;
 Carbodiphosphorane-based nickel pincer complexes and their (de)protonated
 analogues: dimerisation, ligand tautomers and proton affinities.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10544
_journal_page_last               10552
_journal_paper_doi               10.1039/c7dt04930g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C102 H86 Ni2 P8, 2(Cl), 2.5(C H2 Cl2)'
_chemical_formula_sum            'C104.5 H91 Cl7 Ni2 P8'
_chemical_formula_weight         1960.10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-31
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-31 deposited with the CCDC.
2018-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                88.48(3)
_cell_angle_beta                 72.40(3)
_cell_angle_gamma                67.39(3)
_cell_formula_units_Z            2
_cell_length_a                   13.590(3)
_cell_length_b                   17.439(4)
_cell_length_c                   22.442(5)
_cell_measurement_reflns_used    734
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.20
_cell_measurement_theta_min      2.095
_cell_volume                     4656(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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_temperature      100.0
_diffrn_detector                 'image plate'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  IPDS2
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1289
_diffrn_reflns_av_unetI/netI     0.1069
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            41177
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.800
_diffrn_reflns_theta_min         1.675
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       needle
_exptl_crystal_F_000             2026
_exptl_crystal_size_max          0.604
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.194
_refine_diff_density_max         1.431
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         19516
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0641
_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^)+(0.0940P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1638
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13700
_reflns_number_total             19516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04930g2.cif
_cod_data_source_block           intp-1
_cod_depositor_comments
'Adding full bibliography for 7045645--7045649.cif.'
_cod_database_code               7045647
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(Cl2) = Uanis(Cl17)
Uanis(Cl1A) = Uanis(C9) = Uanis(Cl53)
3. Others
 Fixed Sof: Cl2(0.5) Cl17(0.5) Cl21(0.5) Cl53(0.5) Cl19(0.5) C3(0.5) H3A(0.5)
 H3B(0.5) C1(0.5) H1A(0.5) H1B(0.5) Cl1A(0.5) C9(0.5) H9A(0.5) H9B(0.5)
4.a Ternary CH refined with riding coordinates:
 C8(H8), C23(H23)
4.b Secondary CH2 refined with riding coordinates:
 C39(H39A,H39B), C117(H11A,H11B), C171(H17A,H17B), C3(H3A,H3B), C1(H1A,H1B),
 C9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C32(H32), C42(H42), C43(H43), C47(H47), C49(H49), C55(H55),
 C58(H58), C61(H61), C65(H65), C68(H68), C70(H70), C71(H71), C74(H74), C77(H77),
  C79(H79), C84(H84), C85(H85), C88(H88), C92(H92), C94(H94), C96(H96),
 C97(H97), C99(H99), C101(H101), C104(H104), C105(H105), C108(H108), C109(H109),
  C111(H111), C114(H114), C115(H115), C120(H120), C122(H122), C124(H124),
 C125(H125), C127(H127), C130(H130), C131(H131), C134(H134), C136(H136),
 C138(H138), C139(H139), C142(H142), C144(H144), C146(H146), C147(H147),
 C149(H149), C152(H152), C154(H154), C156(H156), C157(H157), C159(H159),
 C162(H162), C163(H163), C166(H166), C168(H168), C169(H169), C173(H173),
 C176(H176), C177(H177), C180(H180), C182(H182), C184(H184), C185(H185),
 C187(H187), C190(H190), C192(H192), C194(H194), C195(H195), C199(H199),
 C202(H202), C204(H204), C206(H206), C208(H208), C210(H210), C211(H211),
 C214(H214), C215(H215), C218(H218)
;
_olex2_submission_special_instructions 'No special instructions were received'