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_4348795
_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_absolute_configuration ad
_chemical_formula_moiety         'F6 Sb, C17 H20.83 Cu N5'
_chemical_formula_sum            'C17 H20.83 Cu F6 N5 Sb'
_chemical_formula_weight         594.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-13
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.6970(13)
_cell_length_b                   8.7362(6)
_cell_length_c                   12.3963(8)
_cell_measurement_reflns_used    9390
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.64
_cell_volume                     2133.1(2)
_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
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0327
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            43702
_diffrn_reflns_theta_full        30.72
_diffrn_reflns_theta_max         30.72
_diffrn_reflns_theta_min         1.64
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.328
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0702 before and 0.0472 after correction.
The Ratio of minimum to maximum transmission is 0.7892.
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    1.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1167
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_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     286
_refine_ls_number_reflns         6616
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0210
_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^)+(0.0167P)^2^+1.2986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0464
_reflns_number_gt                6387
_reflns_number_total             6616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01646_si_004.cif
_cod_data_source_block           fi_abs_lt_ii_51c
_cod_database_code               4348795
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.383(9) 0.617(9)
2. 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
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C16) = Uanis(C16B)
Uanis(C17) = Uanis(C17B)
4. Others
 Sof(H15A)=Sof(C16B)=Sof(H16D)=Sof(H16E)=Sof(H16F)=1-FVAR(1)
 Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(H16C)=FVAR(1)
 Sof(C17)=Sof(H17D)=Sof(H17E)=Sof(H17F)=1-FVAR(2)
 Sof(H15)=Sof(C17B)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C15(H15A), C12(H12)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C5(H5), C8(H8), C9(H9), C10(H10)
5.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C17B(H17A,H17B,H17C), C16(H16A,H16B,
 H16C), C16B(H16D,H16E,H16F), C17(H17D,H17E,H17F)
;
_olex2_submission_special_instructions 'No special instructions were received'