Bimetallic Coordination Insertion Polymerization of Unprotected Polar Monomers: Copolymerization of Amino Olefins and Ethylene by Dinickel Bisphenoxyiminato Catalysts
Madalyn R. Radlauer; Aya K. Buckley; Lawrence M. Henling; Theodor Agapie; Journal of the American Chemical Society 135 (2013) 3784–3787; doi:10.1021/ja4004816

data_4119468
_publ_contact_author_address
;
Beckman Institute
Caltech 139-74
Pasadena CA 91125
USA
;
_publ_contact_author_email       xray@caltech.edu
_publ_contact_author_name        'Xray Staff'
_publ_section_title
;
 Bimetallic Coordination Insertion Polymerization of Unprotected Polar
 Monomers: Copolymerization of Amino Olefins and Ethylene by Dinickel
 Bisphenoxyiminato Catalysts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3784
_journal_page_last               3787
_journal_paper_doi               10.1021/ja4004816
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C64 H94 N2 Ni2 O2 P2'
_chemical_formula_sum            'C86.5 H148 N2 Ni2 O2 P2'
_chemical_formula_weight         1427.42
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2012-12-04
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372),
 SHELXL-2012,
 and manual edit
;
_cell_angle_alpha                104.541(8)
_cell_angle_beta                 90.001(9)
_cell_angle_gamma                116.551(8)
_cell_formula_units_Z            2
_cell_length_a                   13.408(2)
_cell_length_b                   14.878(2)
_cell_length_c                   23.068(4)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.45
_cell_measurement_theta_min      2.35
_cell_volume                     3950.9(11)
_computing_cell_refinement       'SAINT V8.27B (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2012.4-3 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V8.27B (Bruker-AXS, 2007)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
 and SHELXTL (Bruker-AXS, 2007)
;
_computing_structure_refinement  'SHELXL-2012/7 (Sheldrick, 2012)'
_computing_structure_solution
;
SHELXT (Sheldrick, 2012)
PLATON (Spek, 2005)
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.768
_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  0.1141
_diffrn_reflns_av_unetI/netI     0.1828
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.768
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            72075
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.768
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.031
_diffrn_reflns_theta_min         1.601
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.565
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1305 before and 0.1004 after correction.
The Ratio of minimum to maximum transmission is 0.7656.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_description       flake
_exptl_crystal_F_000             1566
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_platon_squeeze_details
;
;
_refine_diff_density_max         6.359
_refine_diff_density_min         -1.537
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.771
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         16211
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.772
_refine_ls_R_factor_all          0.2114
_refine_ls_R_factor_gt           0.1425
_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^)+(0.0800P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3256
_refine_ls_wR_factor_ref         0.3417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7129
_reflns_number_total             16211
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja4004816_si_002.cif
_cod_data_source_block           mrr29
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_source_target' value 'MO' changed to 'Mo' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        3950.8(12)
_cod_original_formula_sum        'C86.50 H148 N2 Ni2 O2 P2'
_cod_database_code               4119468
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H16 of C16, H14 of C14, H21 of C21, H24 of C24, H25 of C25, H26 of C26, H28
  of C28, H31 of C31, H37 of C37, H39 of C39, H44 of C44, H48 of C48, H49 of
  C49, H51 of C51, H54 of C54, H47 of C47
 At 1.5 times of:
  {H63A,H63B,H63C} of C63, {H64A,H64B,H64C} of C64, {H18A,H18B,H18C} of C18,
  {H10A,H10B,H10C} of C10, {H9A,H9B,H9C} of C9, {H8A,H8B,H8C} of C8, {H19A,H19B,
  H19C} of C19, {H20A,H20B,H20C} of C20, {H29A,H29B,H29C} of C29, {H30A,H30B,
  H30C} of C30, {H7A,H7B,H7C} of C7, {H32A,H32B,H32C} of C32, {H33A,H33B,H33C}
  of C33, {H41A,H41B,H41C} of C41, {H42A,H42B,H42C} of C42, {H43A,H43B,H43C} of
  C43, {H62A,H62B,H62C} of C62, {H61A,H61B,H61C} of C61, {H60A,H60B,H60C} of
  C60, {H52A,H52B,H52C} of C52, {H53A,H53B,H53C} of C53, {H55A,H55B,H55C} of
  C55, {H56A,H56B,H56C} of C56, {H57A,H57B,H57C} of C57, {H58A,H58B,H58C} of
  C58, {H59A,H59B,H59C} of C59
2. Uiso/Uaniso restraints and constraints
Uanis(C22) Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3.a Ternary CH refined with riding coordinates:
 C28(H28), C31(H31), C51(H51), C54(H54)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C16(H16), C21(H21), C24(H24), C25(H25), C26(H26), C37(H37),
 C39(H39), C44(H44), C47(H47), C48(H48), C49(H49)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C),
 C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C52(H52A,H52B,H52C),
 C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,
 H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C)
;
_shelx_estimated_absorpt_t_max   0.910
_shelx_estimated_absorpt_t_min   0.840
_shelx_res_checksum              35461
_shelxl_version_number           2012-6