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_7048525
_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 P2 Pd, B0.7 F2.8, 0.3(Cl)'
_chemical_formula_sum            'C30 H30 B0.7 Cl1.3 F2.8 N2 P2 Pd'
_chemical_formula_weight         693.75
_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             2018-06-23
_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                70.883(8)
_cell_angle_beta                 88.024(8)
_cell_angle_gamma                71.058(7)
_cell_formula_units_Z            2
_cell_length_a                   9.4114(14)
_cell_length_b                   12.154(2)
_cell_length_c                   15.368(2)
_cell_measurement_reflns_used    5481
_cell_measurement_temperature    100.15
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      3.371
_cell_volume                     1565.9(4)
_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      100.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Apex3 D8 venture'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12684
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.371
_exptl_absorpt_coefficient_mu    0.845
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0644 before and 0.0378 after correction.
The Ratio of minimum to maximum transmission is 0.9193.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       block
_exptl_crystal_F_000             702
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.737
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         5481
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0370
_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^)+(0.0523P)^2^+1.1423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0962
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4597
_reflns_number_total             5481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03413c2.cif
_cod_data_source_block           PCP-PdBF4
_cod_depositor_comments
'Adding full bibliography for 7048523--7048526.cif.'
_cod_original_cell_volume        1566.0(4)
_cod_original_formula_sum        'C30 H30 B0.70 Cl1.30 F2.80 N2 P2 Pd'
_cod_database_code               7048525
_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
2. Restrained distances
 F1-B2 \\sim F1A-B2
 with sigma of 0.02
 F2-B2 \\sim F2A-B2
 with sigma of 0.02
 F3-B2 \\sim F3A-B2
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 F3, F2, F1, F5, B2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 B2, F2A, F3A, F1A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: F1(0.35) F2(0.35) F3(0.7) F5(0.35) B2(0.7) F1A(0.35) F2A(0.35)
 F3A(0.35) Cl0A(0.3)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C18(H18A,H18B)
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              30014
_olex2_submission_special_instructions 'No special instructions were received'