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_7045645
_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         'C51 H43 Cl Ni P4, 0.5(C4 H8 O)'
_chemical_formula_sum            'C58 H47 Cl Ni O0.5 P4'
_chemical_formula_weight         909.94
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 111.75(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.142(4)
_cell_length_b                   19.799(4)
_cell_length_c                   23.579(5)
_cell_measurement_reflns_used    1891
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     9601(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Stoe 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  0.0867
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            84432
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.797
_diffrn_reflns_theta_min         1.428
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1072
_refine_ls_number_reflns         20237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0492P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0897
_refine_ls_wR_factor_ref         0.0976
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13623
_reflns_number_total             20237
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04930g2.cif
_cod_data_source_block           paper
_cod_depositor_comments
;

2018-02-20
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel

 Adding full bibliography for 7045645--7045649.cif.
;
_cod_original_formula_moiety     '2(C51 H43 Cl Ni P4), C4 H8 O'
_cod_original_formula_sum        'C106 H94 Cl2 Ni2 O P8'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1819.88
_cod_database_code               7045645
_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.a Secondary CH2 refined with riding coordinates:
 C00O(H00A,H00B), C014(H01A,H01B), C031(H03B,H03C), C032(H03D,H03E), C037(H03F,
 H03G), C03B(H03H,H03I)
2.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00L(H00L), C00Q(H00Q), C00R(H00R), C00T(H00T), C00V(H00V),
 C00X(H00X), C00Z(H00Z), C011(H011), C012(H012), C013(H013), C015(H015),
 C016(H016), C017(H017), C018(H018), C01A(H01C), C01B(H01E), C01C(H01F),
 C01D(H01D), C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J), C01K(H01K),
 C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q),
 C01R(H01R), C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V), C01W(H01W),
 C01X(H01X), C01Y(H01Y), C01Z(H01Z), C020(H020), C021(H021), 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),
 C02F(H02F), C02G(H02G), C02H(H02H), 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), C033(H033), C034(H034), C035(H035),
 C036(H036), C038(H038), C039(H039), C03A(H03A)
;
_olex2_submission_special_instructions 'No special instructions were received'