Synthesis of Semicrystalline Polyolefin Materials: Precision Methyl Branching via Stereoretentive Chain Walking.
Vaccarello, David N.; O'Connor, Kyle S; Iacono, Pasquale; Rose, Jeffrey M.; Cherian, Anna E.; Coates, Geoffrey W.; Journal of the American Chemical Society 140 (2018) 6208–6211; doi:10.1021/jacs.8b02963

data_4132325
_publ_section_title
;
 Synthesis of Semicrystalline Polyolefin Materials: Precision Methyl
 Branching via Stereoretentive Chain Walking.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6208
_journal_page_last               6211
_journal_paper_doi               10.1021/jacs.8b02963
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C50 H52 Br2 N2 Ni'
_chemical_formula_sum            'C50 H52 Br2 N2 Ni'
_chemical_formula_weight         899.46
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-05-17
_audit_creation_method
;
Olex2 1.2-ac3
(compiled 2016.08.26 svn.r3337 for Rigaku Oxford Diffraction, GUI svn.r5221)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.1909(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.04574(5)
_cell_length_b                   25.29692(13)
_cell_length_c                   19.03833(11)
_cell_measurement_reflns_used    27324
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      77.6830
_cell_measurement_theta_min      2.9350
_cell_volume                     4241.58(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -57.00  22.00   0.50    1.50    --  -48.05  37.00-120.00  158
  2  \w    -57.00 -29.00   0.50    1.50    --  -48.05 145.00-156.00   56
  3  \w    -59.00  23.00   0.50    1.50    --  -48.05  37.00-180.00  164
  4  \w     48.00  73.00   0.50    1.50    --   48.05-126.00 -41.00   50
  5  \w     94.00 121.00   0.50    5.00    --  107.75-126.00 -41.00   54
  6  \w     81.00 107.00   0.50    5.00    --  107.75 -94.00   0.00   52
  7  \w     81.00 117.00   0.50    5.00    --  107.75 -45.00  90.00   72
  8  \w     80.00 116.00   0.50    5.00    --  107.75 -15.00  60.00   72
  9  \w     98.00 176.00   0.50    5.00    --  107.75  45.00  30.00  156
 10  \w    138.00 168.00   0.50    5.00    --  107.75  45.00   0.00   60
 11  \w    150.00 175.00   0.50    5.00    --  107.75 126.00  35.00   50
 12  \w     97.00 147.00   0.50    5.00    --  107.75 126.00  35.00  100
 13  \w    103.00 156.00   0.50    5.00    --  107.75  61.00 -60.00  106
 14  \w    137.00 171.00   0.50    5.00    --  107.75 125.00-120.00   68
 15  \w    116.00 142.00   0.50    5.00    --  107.75 145.00-156.00   52
 16  \w     95.00 124.00   0.50    5.00    --  107.75 125.00-120.00   58
 17  \w     97.00 132.00   0.50    5.00    --  107.75  45.00   0.00   70
 18  \w     44.00 107.00   0.50    5.00    --  107.75 -61.00 -60.00  126
 19  \w     71.00 103.00   0.50    5.00    --  107.75 -94.00-150.00   64
 20  \w     48.00  74.00   0.50    5.00    --  107.75 -94.00 -60.00   52
 21  \w     39.00 120.00   0.50    5.00    --  107.75 -77.00 -60.00  162
 22  \w     61.00 113.00   0.50    5.00    --  107.75-125.00  90.00  104
 23  \w     72.00  98.00   0.50    1.50    --   48.05-145.00 150.00   52
 24  \w     47.00 107.00   0.50    5.00    --  107.75-145.00 150.00  120
 25  \w     36.00  65.00   0.50    5.00    --  107.75 -45.00  90.00   58
 26  \w     35.00  61.00   0.50    5.00    --  107.75 -15.00  60.00   52
 27  \w   -113.00 -88.00   0.50    1.50    --  -48.05-145.00 150.00   50
 28  \w   -116.00 -76.00   0.50    1.50    --  -48.05-126.00 -41.00   80
 29  \w   -123.00 -97.00   0.50    5.00    --  -86.25-126.00 -41.00   52
 30  \w   -118.00 -78.00   0.50    1.50    --  -48.05-125.00  90.00   80
 31  \w   -132.00-107.00   0.50    5.00    --  -86.25-145.00 150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0078160000
_diffrn_orient_matrix_UB_12      -0.0606384000
_diffrn_orient_matrix_UB_13      0.0055059000
_diffrn_orient_matrix_UB_21      0.0658739000
_diffrn_orient_matrix_UB_22      0.0034223000
_diffrn_orient_matrix_UB_23      0.0819828000
_diffrn_orient_matrix_UB_31      -0.1618626000
_diffrn_orient_matrix_UB_32      0.0043041000
_diffrn_orient_matrix_UB_33      0.0125935000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36578
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.075
_diffrn_reflns_theta_min         2.956
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.134
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.628
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       plate
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.198
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         8040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^+2.7209P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0661
_refine_ls_wR_factor_ref         0.0671
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7606
_reflns_number_total             8040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b02963_si_002.cif
_cod_data_source_block           rdv1_abs2
_cod_database_code               4132325
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C50H52Br2N2Ni
_chemical_oxdiff_usercomment     'Crystallized from DCM/hexanes'
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C11(H11), C12(H12), C22(H22),
 C23(H23), C24(H24), C26(H26), C27(H27), C28(H28), C33(H33), C34(H34), C36(H36),
  C40(H40), C41(H41), C42(H42), C43(H43), C44(H44)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C19(H19A,H19B,H19C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,
 H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C)
;
_shelx_res_checksum              88796
_shelx_hkl_checksum              78687
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.480
_oxdiff_exptl_absorpt_empirical_full_min 0.805