Macrocyclic Aryl‒Nickel(II) Complexes: Synthesis, Structure, and Reactivity Studies
Yang, Chi; Wu, Wen-Di; Zhao, Liang; Wang, Mei-Xiang; Organometallics 34 (2015) 5167–; doi:10.1021/acs.organomet.5b00733

data_4087927
_publ_section_title
;
 Macrocyclic Aryl--Nickel(II) Complexes: Synthesis, Structure, and
 Reactivity Studies
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5167
_journal_paper_doi               10.1021/acs.organomet.5b00733
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C26 H24 N6 Ni'
_chemical_formula_sum            'C26 H24 N6 Ni'
_chemical_formula_weight         479.22
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 106.978(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.248(11)
_cell_length_b                   8.617(3)
_cell_length_c                   21.659(8)
_cell_measurement_reflns_used    8402
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4846
_cell_measurement_theta_min      1.5628
_cell_volume                     4864(3)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2014)'
_computing_structure_solution
;
'SHELXT (Sheldrick, 2014)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
scan:
	Number of images: 180
	           Slice: -110.0000 - 70.0000
	     Image width: 1.0000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.1024
	          2theta: -20.8310
scan:
	Number of images: 179
	           Slice: -110.0000 - 69.0000
	     Image width: 1.0000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.1024
	          2theta: -20.8310
scan:
	Number of images: 174
	           Slice: -110.0000 - 64.0000
	     Image width: 1.0000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 45.1024
	          2theta: -20.8310
scan:
	Number of images: 91
	           Slice: -65.0000 - 26.0000
	     Image width: 1.0000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.1024
	          2theta: -20.8310
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0050
_diffrn_orient_matrix_UB_12      0.0380
_diffrn_orient_matrix_UB_13      0.0023
_diffrn_orient_matrix_UB_21      0.0307
_diffrn_orient_matrix_UB_22      0.0107
_diffrn_orient_matrix_UB_23      -0.1114
_diffrn_orient_matrix_UB_31      -0.0459
_diffrn_orient_matrix_UB_32      0.0089
_diffrn_orient_matrix_UB_33      -0.0118
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0631
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33112
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.494
_diffrn_reflns_theta_min         1.563
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.823
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.260
_refine_diff_density_min         -0.891
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5559
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0885
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1617P)^2^+27.8421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2618
_refine_ls_wR_factor_ref         0.2636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5466
_reflns_number_total             5559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00733_si_002.cif
_cod_data_source_block           Compound4
_cod_database_code               4087927
_diffrn_number_total             5935
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N5-C20
 1.45 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C15(H15), C16(H16),
 C17(H17), C22(H22), C23(H23), C24(H24)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C13(H13A,H13B,H13C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C)
;
_shelx_res_checksum              81821
_shelx_hkl_checksum              27253
_shelx_fab_checksum              17425
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'