Cu(I) Complexes of Pincer Pyridine-Based N-Heterocyclic Carbenes with Small Wingtip Substituents: Synthesis and Structural and Spectroscopic Studies.
Domyati, Doaa; Hope, Sydney L.; Latifi, Reza; Hearns, Micah D.; Tahsini, Laleh; Inorganic chemistry 55 (2016) 11685–11693; doi:10.1021/acs.inorgchem.6b01646

data_4348796
_publ_section_title
;
 Cu(I) Complexes of Pincer Pyridine-Based N-Heterocyclic Carbenes with
 Small Wingtip Substituents: Synthesis and Structural and Spectroscopic
 Studies.
;
_journal_issue                   22
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11685
_journal_page_last               11693
_journal_paper_doi               10.1021/acs.inorgchem.6b01646
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C38 H50 Cu2 N10, 2(F6 P)'
_chemical_formula_sum            'C38 H50 Cu2 F12 N10 P2'
_chemical_formula_weight         1063.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-05-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                80.5870(10)
_cell_angle_beta                 78.9300(10)
_cell_angle_gamma                64.4460(10)
_cell_formula_units_Z            2
_cell_length_a                   11.8254(5)
_cell_length_b                   11.9626(5)
_cell_length_c                   17.9274(7)
_cell_measurement_reflns_used    9823
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.48
_cell_measurement_theta_min      2.31
_cell_volume                     2236.05(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0224
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            69281
_diffrn_reflns_theta_full        28.58
_diffrn_reflns_theta_max         28.58
_diffrn_reflns_theta_min         1.16
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.115
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0528 before and 0.0378 after correction.
The Ratio of minimum to maximum transmission is 0.9091.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.253
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     585
_refine_ls_number_reflns         11303
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+1.8335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0670
_reflns_number_gt                9979
_reflns_number_total             11303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01646_si_005.cif
_cod_data_source_block           dd-2-13b
_cod_database_code               4348796
_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.a Ternary CH refined with riding coordinates:
 C4(H4), C4A(H4A), C17(H17), C17A(H17A)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C8A(H8AA,H8AB), C14(H14A,H14B), C14A(H14C,H14D)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C6A(H6A), C7(H7), C7A(H7A), C10(H10), C10A(H10A), C11(H11),
 C11A(H11A), C12(H12), C12A(H12A), C15(H15), C15A(H15A), C16(H16), C16A(H16A)
2.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC),
 C18(H18A,H18B,H18C), C18A(H18D,H18E,H18F), C19(H19A,H19B,H19C), C19A(H19D,H19E,
 H19F)
;
_olex2_submission_special_instructions 'No special instructions were received'