Facile synthesis of Pd(ii) and Ni(ii) pincer carbene complexes by the double C-H bond activation of a new hexahydropyrimidine-based bis(phosphine): catalysis of C-N couplings.
Subramaniyan, Vasudevan; Dutta, Bidisa; Govindaraj, Anbarasu; Mani, Ganesan; Dalton transactions (Cambridge, England : 2003) 48 (2019) 7203–7210; doi:10.1039/c8dt03413c

data_7048524
_publ_section_title
;
 Facile synthesis of Pd(ii) and Ni(ii) pincer carbene complexes by the
 double C-H bond activation of a new hexahydropyrimidine-based
 bis(phosphine): catalysis of C-N couplings.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7203
_journal_page_last               7210
_journal_paper_doi               10.1039/c8dt03413c
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C30 H30 Cl N2 Ni P2, 1.5(H2 O), Cl'
_chemical_formula_sum            'C30 H33 Cl2 N2 Ni O1.5 P2'
_chemical_formula_weight         637.13
_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   mixed
_audit_creation_date             2018-06-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-23 deposited with the CCDC.
2019-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.366(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.845(3)
_cell_length_b                   9.0434(10)
_cell_length_c                   23.141(3)
_cell_measurement_reflns_used    5177
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.997
_cell_measurement_theta_min      1.44
_cell_volume                     5918.1(12)
_computing_cell_refinement       APEX3
_computing_data_collection       APEX3
_computing_data_reduction        APEX3
_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
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker-D8 Venture APEX3'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0651
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            30717
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.440
_diffrn_source                   'Fine focused sealed tube'
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  0.918
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_description       prism
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.146
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     367
_refine_ls_number_reflns         5177
_refine_ls_number_restraints     17
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0563P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4120
_reflns_number_total             5177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03413c2.cif
_cod_data_source_block           PCP-NiCl2
_cod_depositor_comments
'Adding full bibliography for 7048523--7048526.cif.'
_cod_original_cell_volume        5918.2(11)
_cod_original_formula_sum        'C30 H33 Cl2 N2 Ni O1.50 P2'
_cod_database_code               7048524
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C14-C15 \\sim C14-C15A
 with sigma of 0.02
 C15-C16 \\sim C15A-C16
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C16, C15, C15A, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H14C)=Sof(H14D)=Sof(H16C)=Sof(H16D)=Sof(C15A)=Sof(H15C)=Sof(H15D)=1-FVAR(1)
 Sof(H14A)=Sof(H14B)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H16A)=Sof(H16B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C14(H14C,H14D), C15(H15A,H15B), C16(H16A,
 H16B), C16(H16C,H16D), C18(H18A,H18B), C15A(H15C,H15D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27),
  C28(H28), C29(H29), C30(H30)
;
_shelx_res_checksum              43988
_olex2_submission_special_instructions 'No special instructions were received'