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_7045646
_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         'C52 H47 Ni P4, C2 H6 Al Cl2'
_chemical_formula_sum            'C54 H53 Al Cl2 Ni P4'
_chemical_formula_weight         982.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 108.4890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3928(6)
_cell_length_b                   20.9075(10)
_cell_length_c                   18.7057(11)
_cell_measurement_reflns_used    9936
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.352
_cell_measurement_theta_min      2.261
_cell_volume                     4967.4(4)
_computing_cell_refinement       'APEX3 v2016.1-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v3.0.26'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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                 'Photon 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_detector_type            'CMOS active pixel sensor'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'fixed-chi goniometer'
_diffrn_measurement_device_type  'D8 Quest (Bruker AXS Inc.)'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0519
_diffrn_reflns_av_unetI/netI     0.0301
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26730
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.392
_diffrn_reflns_theta_max         24.392
_diffrn_reflns_theta_min         2.261
_diffrn_source                   'I\mS Microfocus Source'
_diffrn_source_type              'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.680
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6697
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1115 before and 0.0551 after correction. The Ratio of minimum to maximum transmission is 0.8988. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.263
_exptl_crystal_size_min          0.211
_refine_diff_density_max         0.372
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0269P)^2^+12.4370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3442
_reflns_number_total             4055
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04930g2.cif
_cod_data_source_block           lmcdp100_0ma_a
_cod_depositor_comments
'Adding full bibliography for 7045645--7045649.cif.'
_cod_database_code               7045646
_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. Others
 Fixed Sof: H00V(0.5) H00W(0.5) H00X(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C008(H00A,H00B)
3.b Aromatic/amide H refined with riding coordinates:
 C00C(H00C), C00D(H00D), C00E(H00E), C00F(H00F), C00G(H00G), C00H(H00H),
 C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M), C00N(H00N),
 C00O(H00O), C00P(H00P), C00Q(H00Q), C00R(H00R), C00S(H00S), C00T(H00T),
 C00U(H00U), C00W(H00Y)
3.c Idealised Me refined as rotating group:
 C00V(H00V,H00W,H00X), C00X(H00Z,H,HA)
;
_audit_contact_author            'L. Maser'
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'