Homo- and copolymerization of norbornene with tridentate nickel complexes bearing o-aryloxide-N-heterocyclic carbene ligands.
Yang, Dandan; Dong, Jie; Wang, Baiquan; Dalton transactions (Cambridge, England : 2003) 47 (2018) 180–189; doi:10.1039/c7dt03928j

data_7044829
_publ_section_title
;
 Homo- and copolymerization of norbornene with tridentate nickel complexes
 bearing o-aryloxide-N-heterocyclic carbene ligands.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              180
_journal_page_last               189
_journal_paper_doi               10.1039/c7dt03928j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C46 H56 N6 Ni O2, 2(C H2 Cl2)'
_chemical_formula_sum            'C48 H60 Cl4 N6 Ni O2'
_chemical_formula_weight         953.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2017-07-06 deposited with the CCDC.
2017-11-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.097(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4152(16)
_cell_length_b                   14.2949(15)
_cell_length_c                   24.256(2)
_cell_measurement_reflns_used    15400
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.0
_cell_volume                     4868.3(8)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalClear
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku Saturn 724CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0566
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44741
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.906
_diffrn_reflns_theta_min         1.724
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.901
_exptl_absorpt_correction_T_min  0.858
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.341
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         11589
_refine_ls_number_restraints     232
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0804
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+5.9496P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1879
_refine_ls_wR_factor_ref         0.1975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9887
_reflns_number_total             11589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03928j2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7044828--7044829.cif.'
_cod_original_cell_volume        4868.3(9)
_cod_database_code               7044829
_shelx_shelxl_version_number     2014/8
_shelx_estimated_absorpt_t_max   0.902
_shelx_estimated_absorpt_t_min   0.857
_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 C(H,H,H) groups
2. Restrained distances
 C34-C35 = C34-C36 = C34-C37 = C34-C35' = C34-C36' = C34-C37'
 1.54 with sigma of 0.01
 Cl1-C47 = Cl2-C47 = Cl1'-C47' = Cl2'-C47'
 1.72 with sigma of 0.01
 Cl3-C48 = Cl4-C48 = Cl3'-C48' = Cl4'-C48' = Cl3"-C48" = Cl4"-C48"
 1.72 with sigma of 0.01
 Cl1-Cl2 = Cl3-Cl4
 2.8 with sigma of 0.01
 C35-C36 \\sim C35-C37 \\sim C36-C37 \\sim C35'-C36' \\sim C35'-C37' \\sim
C36'-C37'
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C35')
\\sim Ueq, Uanis(C36') \\sim Ueq, Uanis(C37') \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C42) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(N6) \\sim Ueq, Uanis(C42') \\sim Ueq,
Uanis(N6') \\sim Ueq, Uanis(C44') \\sim Ueq, Uanis(C45') \\sim Ueq, Uanis(C46')
\\sim Ueq, Uanis(C43') \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C47) \\sim Ueq, Uanis(Cl1')
\\sim Ueq, Uanis(Cl2') \\sim Ueq, Uanis(C47') \\sim Ueq, Uanis(Cl3) \\sim Ueq,
Uanis(Cl4) \\sim Ueq, Uanis(C48) \\sim Ueq, Uanis(Cl3') \\sim Ueq, Uanis(Cl4')
\\sim Ueq, Uanis(C48') \\sim Ueq, Uanis(Cl3") \\sim Ueq, Uanis(Cl4") \\sim Ueq,
Uanis(C48") \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C42) = Uanis(C42')
4. Others
 1*[Sof(Cl3)+Sof(Cl4)+Sof(C48)+Sof(H48A)+Sof(H48B)]+1*[Sof(Cl3')+Sof(Cl4')+
 Sof(C48')+Sof(H48C)+Sof(H48D)]+1*[Sof(Cl3")+Sof(Cl4")+Sof(C48")+Sof(H48E)+
 Sof(H48F)]=1 with esd of 0.0001
 Sof(H41C)=Sof(H41D)=Sof(C42')=Sof(N6')=Sof(C44')=Sof(H44')=Sof(C45')=
 Sof(H45')=Sof(C46')=Sof(H46')=Sof(C43')=Sof(H43')=1-FVAR(1)
 Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=
 Sof(H45)=Sof(C46)=Sof(H46)=Sof(N6)=FVAR(1)
 Sof(C35')=Sof(H35D)=Sof(H35E)=Sof(H35F)=Sof(C36')=Sof(H36D)=Sof(H36E)=
 Sof(H36F)=Sof(C37')=Sof(H37D)=Sof(H37E)=Sof(H37F)=1-FVAR(2)
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=FVAR(2)
 Sof(Cl1')=Sof(Cl2')=Sof(C47')=Sof(H47C)=Sof(H47D)=1-FVAR(3)
 Sof(Cl1)=Sof(Cl2)=Sof(C47)=Sof(H47A)=Sof(H47B)=FVAR(3)
 Sof(Cl3)=Sof(Cl4)=Sof(C48)=Sof(H48A)=Sof(H48B)=FVAR(4)
 Sof(Cl3')=Sof(Cl4')=Sof(C48')=Sof(H48C)=Sof(H48D)=FVAR(5)
 Sof(Cl3")=Sof(Cl4")=Sof(C48")=Sof(H48E)=Sof(H48F)=FVAR(6)
5.a Riding coordinates:
 C41(H41A,H41B,H41C,H41D), C43(H43), C44(H44), C45(H45), C46(H46), C44'(H44'),
 C45'(H45'), C46'(H46')
5.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C47(H47A,H47B), C47'(H47C,H47D), C48(H48A,H48B), C48'(H48C,
 H48D), C48"(H48E,H48F)
5.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C6(H6), C15(H15), C16(H16), C20(H20), C21(H21), C22(H22), C23(H23),
 C26(H26), C28(H28), C38(H38), C39(H39), C43'(H43')
5.d Fitted hexagon refined as free rotating group:
 C42(C43,C44,C45,C46,N6), C42'(N6',C44',C45',C46',C43')
5.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C31(H31A,H31B,H31C), C32(H32A,H32B,
 H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C35'(H35D,H35E,H35F), C36'(H36D,H36E,H36F), C37'(H37D,H37E,H37F)
;
_shelx_res_checksum              61269
_olex2_submission_special_instructions 'No special instructions were received'