Crystalline Coordination Networks of Zero-Valent Metal Centers: Formation of a 3-Dimensional Ni(0) Framework with m-Terphenyl Diisocyanides.
Agnew, Douglas W.; DiMucci, Ida M.; Arroyave, Alejandra; Gembicky, Milan; Moore, Curtis E.; MacMillan, Samantha N.; Rheingold, Arnold L.; Lancaster, Kyle M.; Figueroa, Joshua S.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b09569

data_4126745
_publ_section_title
;
 Crystalline Coordination Networks of Zero-Valent Metal Centers: Formation
 of a 3-Dimensional Ni(0) Framework with m-Terphenyl Diisocyanides.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b09569
_journal_year                    2017
_chemical_formula_moiety
'C100.04 H96.12 N4 Ni, 0.5(C25 H24 N), C1.75 H3.5 O0.5'
_chemical_formula_sum            'C114.29 H111.62 N4.5 Ni O0.5'
_chemical_formula_weight         1614.88
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-01-30
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                90
_cell_angle_beta                 124.556(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   29.5994(12)
_cell_length_b                   34.1170(11)
_cell_length_c                   25.9158(9)
_cell_measurement_reflns_used    2236
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      41.17
_cell_measurement_theta_min      2.23
_cell_volume                     21553.6(14)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2016)'
_computing_data_collection       'APEX3 v2016.9-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2016)'
_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      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.1341
_diffrn_reflns_av_unetI/netI     0.1385
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33502
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        50.589
_diffrn_reflns_theta_max         50.589
_diffrn_reflns_theta_min         2.227
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker MicroStar FR-592'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.595
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.6164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0675 before and 0.0489 after correction. The Ratio of minimum to maximum transmission is 0.8219. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.995
_exptl_crystal_description       block
_exptl_crystal_F_000             6887
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.730
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1086
_refine_ls_number_reflns         11351
_refine_ls_number_restraints     1073
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.1928
_refine_ls_R_factor_gt           0.0982
_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^)+(0.1781P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2507
_refine_ls_wR_factor_ref         0.3121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5291
_reflns_number_total             11351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09569_si_002.cif
_cod_data_source_block           jfigcu123_a_sq_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_formula_sum        'C114.29 H111.62 N4.50 Ni O0.50'
_cod_database_code               4126745
_shelx_shelxl_version_number     2016/6
_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. Restrained distances
 C22L-C21L
 1.539 with sigma of 0.02
 O1-C4S
 1.4 with sigma of 0.02
 O1-C1S
 1.4 with sigma of 0.02
 C3S-C4S
 1.5 with sigma of 0.02
 C3S-C2S
 1.5 with sigma of 0.02
 C1S-C2S
 1.5 with sigma of 0.02
 C1S-C3S
 2.5 with sigma of 0.02
 C4S-C2S
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C34) = Uanis(C35A)
Uanis(C33) = Uanis(C34A)
Uanis(C32) = Uanis(C33A)
Uanis(C35) = Uanis(C36A)
Uanis(C31) = Uanis(C31A)
Uanis(C36) = Uanis(C37A)
Uanis(C37) = Uanis(C38A)
Uanis(C30) = Uanis(C30A)
Uanis(C32A) = Uanis(C99)
Uanis(C57) = Uanis(C57B)
Uanis(C58) = Uanis(C58B)
Uanis(C59) = Uanis(C59B)
Uanis(C56) = Uanis(C63B) = Uanis(C56B)
Uanis(C55) = Uanis(C55B)
Uanis(C61) = Uanis(C61B)
Uanis(C60) = Uanis(C58B) = Uanis(C60B)
Uanis(C63B) = Uanis(C63)
Uanis(C56) = Uanis(C56B)
Uanis(C62A) = Uanis(C62B)
Uanis(C51) = Uanis(C51A)
Uanis(C50) = Uanis(C50A)
Uanis(C52) = Uanis(C52A)
Uanis(C53) = Uanis(C53A)
Uanis(C54) = Uanis(C54A)
Uanis(C46) = Uanis(C46A)
Uanis(C47) = Uanis(C47A)
Uanis(C49) = Uanis(C49A)
Uanis(C48) = Uanis(C48A)
Uanis(C98) = Uanis(C15A)
Uanis(C14) = Uanis(C14A)
Uanis(C1L) = Uanis(N5) = Uanis(C2L) = Uanis(C4L) = Uanis(C5L) = Uanis(C6L) =
Uanis(C7L) = Uanis(C3L) = Uanis(C10L) = Uanis(C9L) = Uanis(C8L) = Uanis(C15L) =
Uanis(C16L) = Uanis(C14L) = Uanis(C12L) = Uanis(C11L) = Uanis(C13L) =
Uanis(C17L) = Uanis(C24L) = Uanis(C25L) = Uanis(C23L) = Uanis(C21L) =
Uanis(C20L) = Uanis(C18L) = Uanis(C19L) = Uanis(C22L)
Uanis(C3S) = Uanis(C2S) = Uanis(C1S) = Uanis(O1) = Uanis(C4S)
4. Rigid body (RIGU) restrains
 Ni1, N4, N3, N1, N2, C89, C66, C80, C18, C3, C79, C5, C68, C2, C67, C65, C19,
 C15, C1, C88, C90, C17, C6, C20, C4, C100, C7, C16, C8, C86, C40, C64, C96,
 C41, C39, C95, C93, C21, C70, C43, C44, C69, C42, C82, C72, C45, C71, C01C,
 C85, C28, C77, C78, C13, C92, C87, C30, C11, C81, C83, C22, C91, C73, C9, C10,
 C46A, C29, C94, C53A, C76, C24, C97, C25, C47A, C31, C49A, C50A, C74, C23, C27,
  C37A, C12, C14, C84, C54A, C33A, C35, C36, C99, C75, C26, C15A, C52A, C32,
 C48A, C51A, C98, C14A, C34, C36A, C38A, C33, C35A, C31A, C30A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C53, C53A, C54, C54A, C46A, C46, C47A, C47, C1L, C48A, C49, C49A, C50, C50A,
 C51, C51A, C52, C52A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22L, C21L, C23L, C20L, C18L, C17L, C24L, C25L, C19L
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C7L, C6L, C2L, C3L, C4L, C5L
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C15L, C14L, C12L, C13L, C11L, C9L, C8L, C10L, C16L
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C80, C79, C86, C82, C85, C87, C81, C83, C84, C66, C68, C67, C65, C64, C69,
 C70, C72, C71, C73, C76, C74, C75, C77, C78
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22L, C21L, C20L, C23L, C24L, C17L, C18L, C19L, C25L
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C30)=Sof(C31)=Sof(C32)=Sof(H32)=Sof(C33)=Sof(C35)=Sof(H35)=Sof(C36)=
 Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(H99C)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=1-FVAR(1)
 Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C35A)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=Sof(C34A)=Sof(C33A)=Sof(H33A)=Sof(C31A)=Sof(C30A)=Sof(C37A)=
 Sof(C36A)=Sof(H36A)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
 Sof(C50A)=Sof(C52A)=Sof(H52A)=Sof(C53A)=Sof(C46A)=Sof(C47A)=Sof(C49A)=
 Sof(H49A)=Sof(C54A)=Sof(H54A)=Sof(H54B)=Sof(H54C)=Sof(C48A)=Sof(H48A)=
 Sof(H48B)=Sof(H48C)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(H51C)=1-FVAR(2)
 Sof(C54)=Sof(H54D)=Sof(H54E)=Sof(H54F)=Sof(C49)=Sof(H49)=Sof(C50)=Sof(C52)=
 Sof(H52)=Sof(C53)=Sof(C46)=Sof(C47)=Sof(C51)=Sof(H51D)=Sof(H51E)=Sof(H51F)=
 Sof(C48)=Sof(H48D)=Sof(H48E)=Sof(H48F)=FVAR(2)
 Sof(C58)=Sof(C57)=Sof(H57)=Sof(C56)=Sof(C55)=Sof(C61)=Sof(C60)=Sof(H60)=
 Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(H59C)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(H63C)=
 Sof(C62A)=Sof(H62D)=Sof(H62E)=Sof(H62F)=1-FVAR(3)
 Sof(C62B)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(C58B)=Sof(C57B)=Sof(H57B)=
 Sof(C56B)=Sof(C55B)=Sof(C61B)=Sof(C60B)=Sof(H60B)=Sof(C59B)=Sof(H59D)=
 Sof(H59E)=Sof(H59F)=Sof(C63B)=Sof(H63D)=Sof(H63E)=Sof(H63F)=FVAR(3)
 Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(H98C)=FVAR(4)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=1-FVAR(5)
 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=FVAR(5)
 Fixed Sof: C15A(0.64109) H15A(0.64109) H15B(0.64109) H15C(0.64109) C23L(0.5)
 H23L(0.5) C24L(0.5) C17L(0.5) C18L(0.5) C20L(0.5) H20L(0.5) C21L(0.5)
 C25L(0.5) H25A(0.5) H25B(0.5) H25C(0.5) C19L(0.5) H19A(0.5) H19B(0.5)
 H19C(0.5) C15L(0.5) C14L(0.5) H14L(0.5) C11L(0.5) H11L(0.5) C8L(0.5) C9L(0.5)
 C12L(0.5) C16L(0.5) H16A(0.5) H16B(0.5) H16C(0.5) N5(0.5) C4L(0.5) H4L(0.5)
 C7L(0.5) C2L(0.5) C13L(0.5) H13A(0.5) H13B(0.5) H13C(0.5) C3L(0.5) C10L(0.5)
 H10A(0.5) H10B(0.5) H10C(0.5) C5L(0.5) C6L(0.5) H6L(0.5) C1L(0.5) C22L(0.5)
 H22A(0.5) H22B(0.5) H22C(0.5) O1(0.5) C1S(0.5) H1SA(0.5) H1SB(0.5) C4S(0.5)
 H4SA(0.5) H4SB(0.5) C2S(0.25) H2SA(0.25) H2SB(0.25) C3S(0.5) H3SA(0.5)
 H3SB(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C4S(H4SA,H4SB), C2S(H2SA,H2SB), C3S(H3SA,H3SB)
6.b Me refined with riding coordinates:
 C59B(H59D,H59E,H59F), C22L(H22A,H22B,H22C)
6.c Aromatic/amide H refined with riding coordinates:
 C65(H65), C6(H6), C20(H20), C4(H4), C16(H16), C95(H95), C44(H44), C69(H69),
 C42(H42), C82(H82), C85(H85), C13(H13), C92(H92), C32(H32), C35(H35), C73(H73),
  C10(H10), C76(H76), C24(H24), C52A(H52A), C49A(H49A), C27(H27), C23L(H23L),
 C20L(H20L), C14L(H14L), C11L(H11L), C4L(H4L), C6L(H6L), C33A(H33A), C36A(H36A),
  C57(H57), C60(H60), C57B(H57B), C60B(H60B), C49(H49), C52(H52)
6.d Fitted hexagon refined as free rotating group:
 C30(C31,C32,C33,C35,C36), C50A(C52A,C53A,C46A,C47A,C49A), C23L(C24L,C17L,C18L,
 C20L,C21L), C34A(C33A,C31A,C30A,C37A,C36A), C58(C57,C56,C55,C61,C60),
 C58B(C57B,C56B,C55B,C61B,C60B), C49(C50,C52,C53,C46,C47)
6.e Idealised Me refined as rotating group:
 C72(H72A,H72B,H72C), C78(H78A,H78B,H78C), C87(H87A,H87B,H87C), C81(H81A,H81B,
 H81C), C91(H91A,H91B,H91C), C29(H29A,H29B,H29C), C94(H94A,H94B,H94C), C97(H97A,
 H97B,H97C), C23(H23A,H23B,H23C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C),
 C84(H84A,H84B,H84C), C54A(H54A,H54B,H54C), C99(H99A,H99B,H99C), C75(H75A,H75B,
 H75C), C26(H26A,H26B,H26C), C15A(H15A,H15B,H15C), C48A(H48A,H48B,H48C),
 C51A(H51A,H51B,H51C), C25L(H25A,H25B,H25C), C19L(H19A,H19B,H19C), C16L(H16A,
 H16B,H16C), C13L(H13A,H13B,H13C), C10L(H10A,H10B,H10C), C98(H98A,H98B,H98C),
 C14A(H14D,H14E,H14F), C34(H34A,H34B,H34C), C38A(H38A,H38B,H38C), C35A(H35A,
 H35B,H35C), C37(H37A,H37B,H37C), C32A(H32A,H32B,H32C), C62B(H62A,H62B,H62C),
 C59(H59A,H59B,H59C), C63(H63A,H63B,H63C), C63B(H63D,H63E,H63F), C62A(H62D,H62E,
 H62F), C54(H54D,H54E,H54F), C51(H51D,H51E,H51F), C48(H48D,H48E,H48F)
;
_shelx_res_checksum              1305
_shelx_hkl_checksum              71507
_shelx_fab_checksum              15435
_olex2_submission_original_sample_id JFigCu123
_olex2_submission_special_instructions 'No special instructions were received'