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_4126746
_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 H100 N4 Ni, C F3 O3 S, C7 H8'
_chemical_formula_sum            'C108 H108 F3 N4 Ni O3 S'
_chemical_formula_weight         1657.75
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-11-25
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.939(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.5352(6)
_cell_length_b                   21.4824(9)
_cell_length_c                   24.9074(11)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      2.34
_cell_volume                     8814.7(6)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Apex-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0818
_diffrn_reflns_av_unetI/netI     0.0901
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            68838
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         25.489
_diffrn_reflns_theta_min         1.236
_exptl_absorpt_coefficient_mu    0.306
_exptl_absorpt_correction_T_max  0.4901
_exptl_absorpt_correction_T_min  0.4404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0716 before and 0.0473 after correction.
The Ratio of minimum to maximum transmission is 0.8986.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'dull light yellow'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_description       block
_exptl_crystal_F_000             3516
_exptl_crystal_recrystallization_method 'saturated toluene solution at -35C'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.791
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1106
_refine_ls_number_reflns         16252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1421
_refine_ls_R_factor_gt           0.0676
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+8.0813P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1926
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9073
_reflns_number_total             16252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09569_si_002.cif
_cod_data_source_block           jfig1249_0m_a
_cod_database_code               4126746
_shelxl_version_number           2013-2
_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.a Aromatic/amide H refined with riding coordinates:
 C00H(H00H), C00W(H00W), C014(H014), C015(H015), C019(H019), C01C(H01C),
 C01F(H01F), C01K(H01K), C01N(H01N), C01Q(H01Q), C01T(H01T), C01W(H01W),
 C01X(H01X), C01Y(H01Y), C01Z(H01Z), C021(H021), C023(H023), C025(H025),
 C026(H026), C027(H027), C028(H028), C02C(H02G), C02J(H02T), C02L(H02U),
 C02N(H02Y), C02P(H02), C02Q(H0AA), C02T(H6AA), C02U(H3AA), C02Y(H7AA),
 C02Z(H8AA), C034(H034), C035(H035)
2.b Idealised Me refined as rotating group:
 C01J(H01A,H01B,H01D), C01M(H01E,H01G,H01H), C029(H02A,H02B,H02C), C02A(H02D,
 H02E,H02F), C02D(H02H,H02I,H02J), C02E(H02K,H02L,H02M), C02F(H02N,H02O,H02P),
 C02G(H02Q,H02R,H02S), C02M(H02V,H02W,H02X), C02O(H02Z,H,HA), C02R(H1AA,HB,HC),
 C02S(H2AA,HD,HE), C02W(H4AA,HF,HG), C02X(H5AA,HH,HI), C030(H03A,H03B,H03C),
 C031(H03D,H03E,H03F), C032(H03G,H03H,H03I), C033(H03J,H03K,H03L), C036(H03M,
 H03N,H03O), C037(H03P,H03Q,H03R), C038(H03S,H03T,H03U), C039(H03V,H03W,H03X),
 C03A(H03Y,HJ,HK), C03B(H03Z,HL,HM), C03C(H03,HN,HO)
;
_shelx_res_checksum              71819
_shelx_hkl_checksum              72743
_olex2_submission_special_instructions 'No special instructions were received'