Nickel-metalated porous organic polymer for Suzuki–Miyaura cross-coupling reaction
Dong, Ying; Jv, Jing-Jing; Li, Yue; Li, Wen-Han; Chen, Yun-Qi; Sun, Qian; Ma, Jian-Ping; Dong, Yu-Bin; RSC Advances 9 (2019) 20266–; doi:10.1039/C9RA03679B

data_7232989
_publ_section_title
;
 Nickel-metalated porous organic polymer for Suzuki--Miyaura
 cross-coupling reaction
;
_journal_issue                   35
_journal_name_full               'RSC Advances'
_journal_page_first              20266
_journal_paper_doi               10.1039/C9RA03679B
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C28 H38 I2 N2'
_chemical_formula_sum            'C28 H38 I2 N2'
_chemical_formula_weight         656.40
_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
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-03-15
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:54:37, GUI svn.r4466)
;
_audit_update_record
;
2019-03-30 deposited with the CCDC.    2019-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 105.541(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6628(3)
_cell_length_b                   17.8319(5)
_cell_length_c                   8.5916(3)
_cell_measurement_reflns_used    2737
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      70.8330
_cell_measurement_theta_min      7.8740
_cell_volume                     1426.26(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
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.
;
_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.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0793
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9989
_diffrn_measured_fraction_theta_max 0.9787
_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     30.00  56.00   1.00    1.00    --    0.00  57.00  90.00   26
  2  \w     37.00  69.00   1.00    1.00    --    0.00  57.00 120.00   32
  3  \w     26.00 123.00   1.00    1.00    --   54.00  77.00 150.00   97
  4  \w     32.00  68.00   1.00    1.00    --   54.00 -57.00 150.00   36
  5  \w     43.00 138.00   1.00    1.00    --  108.00 -77.00 120.00   95
  6  \w     83.00 110.00   1.00    1.00    --  108.00-111.00  90.00   27
  7  \w     69.00 102.00   1.00    1.00    --   54.00-125.00  30.00   33
  8  \w     47.00  84.00   1.00    1.00    --  108.00-111.00 120.00   37
  9  \w     38.00  77.00   1.00    1.00    --  108.00-111.00  90.00   39
 10  \w     -4.00  72.00   1.00    1.00    --   54.00 -57.00  30.00   76
 11  \w     92.00 140.00   1.00    1.00    --  108.00 -25.00 -90.00   48
 12  \w     85.00 111.00   1.00    1.00    --   54.00  57.00-150.00   26
 13  \w    112.00 175.00   1.00    1.00    --  108.00  77.00-120.00   63
 14  \w    103.00 153.00   1.00    1.00    --  108.00 111.00 -60.00   50
 15  \w     36.00 141.00   1.00    1.00    --  108.00 -25.00-180.00  105
 16  \w     89.00 114.00   1.00    1.00    --  108.00-111.00-180.00   25
 17  \w     38.00  63.00   1.00    1.00    --  108.00 -25.00 -90.00   25
 18  \w    -20.00   7.00   1.00    1.00    --    0.00  57.00 120.00   27
 19  \w    -14.00  13.00   1.00    1.00    --    0.00  57.00  90.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0978980000
_diffrn_orient_matrix_UB_12      0.0697084000
_diffrn_orient_matrix_UB_13      0.0280966000
_diffrn_orient_matrix_UB_21      0.1333768000
_diffrn_orient_matrix_UB_22      -0.0509707000
_diffrn_orient_matrix_UB_23      0.0504182000
_diffrn_orient_matrix_UB_31      0.0068127000
_diffrn_orient_matrix_UB_32      -0.0034601000
_diffrn_orient_matrix_UB_33      -0.1767797000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0861
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            5003
_diffrn_reflns_theta_full        67.00
_diffrn_reflns_theta_max         67.02
_diffrn_reflns_theta_min         4.75
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.429
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.317
_refine_diff_density_min         -2.204
_refine_diff_density_rms         0.314
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0902
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1874P)^2^+0.3721P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2424
_refine_ls_wR_factor_ref         0.2483
_reflns_number_gt                2299
_reflns_number_total             2547
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ra03679b2.cif
_cod_data_source_block           11
_cod_database_code               7232989
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 Ternary CH refined with riding coordinates:
 C2(H2), C10(H10)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C)
;
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.892
_oxdiff_exptl_absorpt_empirical_full_min 0.365