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_7045649
_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         '3(C102 H84 Ni2 P8), C4 H8 O, 1.5(C6 H14)'
_chemical_formula_sum            'C319 H281 Ni6 O P24'
_chemical_formula_weight         5225.96
_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   mixed
_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                91.13(3)
_cell_angle_beta                 97.92(3)
_cell_angle_gamma                119.53(3)
_cell_formula_units_Z            1
_cell_length_a                   14.102(3)
_cell_length_b                   14.186(3)
_cell_length_c                   39.126(8)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     6710(3)
_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 0.992
_diffrn_measured_fraction_theta_max 0.982
_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  0.0695
_diffrn_reflns_av_unetI/netI     0.1364
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            80180
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.772
_diffrn_reflns_theta_min         1.585
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.613
_exptl_absorpt_correction_T_max  0.9574
_exptl_absorpt_correction_T_min  0.8758
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_description       plate
_exptl_crystal_F_000             2731
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.178
_exptl_crystal_size_min          0.071
_refine_diff_density_max         1.045
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.842
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1584
_refine_ls_number_reflns         28059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.842
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0566P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1378
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13130
_reflns_number_total             28059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04930g2.cif
_cod_data_source_block           abskorr
_cod_depositor_comments
'Adding full bibliography for 7045645--7045649.cif.'
_cod_database_code               7045649
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C04X) = Uanis(C04V) = Uanis(C04Z) = Uanis(O04Q) = Uanis(C04Y)
Uanis(C9) = Uanis(C7) = Uanis(C6) = Uanis(C8) = Uanis(C10) = Uanis(C11)
3. Others
 Fixed Sof: O04Q(0.5) C04V(0.5) H04P(0.5) H04Q(0.5) C04X(0.5) H04R(0.5)
 H04S(0.5) C04Y(0.5) H04T(0.5) H04U(0.5) C04Z(0.5) H04V(0.5) H04W(0.5) C6(0.75)
 H6A(0.75) H6B(0.75) C7(0.75) H7A(0.75) H7B(0.75) C8(0.75) H8A(0.75) H8B(0.75)
 C9(0.75) H9A(0.75) H9B(0.75) H9C(0.75) C10(0.75) H10A(0.75) H10B(0.75)
 C11(0.75) H11A(0.75) H11B(0.75) H11C(0.75)
4.a Secondary CH2 refined with riding coordinates:
 C04V(H04P,H04Q), C04X(H04R,H04S), C04Y(H04T,H04U), C04Z(H04V,H04W), C6(H6A,
 H6B), C7(H7A,H7B), C8(H8A,H8B), C10(H10A,H10B)
4.b Aromatic/amide H refined with riding coordinates:
 C00N(H00N), C00U(H00U), C00V(H00V), C00Y(H00Y), C010(H010), C011(H011),
 C014(H014), C015(H015), C017(H017), C018(H018), C01C(H01C), C01D(H01D),
 C01E(H01E), C01F(H01F), C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J),
 C01K(H01K), C01M(H01M), C01O(H01O), C01P(H01P), C01R(H01R), C01S(H01S),
 C01T(H01T), C01U(H01U), C01V(H01V), C01W(H01W), C01Y(H01Y), C01Z(H01Z),
 C022(H022), C023(H023), C024(H024), C025(H025), C026(H026), C027(H027),
 C028(H028), C029(H029), C02A(H02A), C02B(H02B), C02C(H02C), C02D(H02D),
 C02E(H02E), C02I(H02I), C02J(H02J), C02K(H02K), C02L(H02L), C02M(H02M),
 C02N(H02N), C02O(H02O), C02P(H02P), C02Q(H02Q), C02R(H02R), C02S(H02S),
 C02T(H02T), C02U(H02U), C02V(H02V), C02W(H02W), C02X(H02X), C02Y(H02Y),
 C02Z(H02Z), C030(H030), C031(H031), C032(H032), C033(H033), C034(H034),
 C035(H035), C036(H036), C037(H037), C038(H038), C039(H039), C03A(H03A),
 C03B(H03B), C03C(H03C), C03D(H03D), C03E(H03E), C03F(H03F), C03G(H03G),
 C03H(H03H), C03I(H03I), C03J(H03J), C03K(H03K), C03L(H03L), C03M(H03M),
 C03N(H03N), C03P(H03P), C03Q(H03Q), C03R(H03R), C03S(H03S), C03T(H03T),
 C03U(H03U), C03V(H03V), C03W(H03W), C03X(H03X), C03Y(H03Y), C03Z(H03Z),
 C040(H040), C041(H041), C042(H042), C043(H043), C044(H044), C045(H045),
 C046(H046), C047(H047), C048(H048), C04A(H04A), C04B(H04B), C04C(H04C),
 C04D(H04D), C04E(H04E), C04F(H04F), C04G(H04G), C04H(H04H), C04I(H04I),
 C04J(H04J), C04K(H04K), C04L(H04L), C04M(H04M), C04N(H04N), C04O(H04O)
4.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
;
_olex2_submission_special_instructions 'No special instructions were received'