Cu(II) Coordination Polymers as Vehicles in the A(3) Coupling.
Loukopoulos, Edward; Kallitsakis, Michael; Tsoureas, Nikolaos; Abdul-Sada, Alaa; Chilton, Nicholas F.; Lykakis, Ioannis N.; Kostakis, George E.; Inorganic chemistry 56 (2017) 4898–4910; doi:10.1021/acs.inorgchem.6b03084

data_4345813
_publ_section_title
;
 Cu(II) Coordination Polymers as Vehicles in the A(3) Coupling.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4898
_journal_page_last               4910
_journal_paper_doi               10.1021/acs.inorgchem.6b03084
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C44 H38 N14 Zn'
_chemical_formula_sum            'C44 H38 N14 Zn'
_chemical_formula_weight         828.25
_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
_audit_creation_date             2017-02-13
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_cell_angle_alpha                108.539(5)
_cell_angle_beta                 95.030(4)
_cell_angle_gamma                101.159(4)
_cell_formula_units_Z            1
_cell_length_a                   9.1257(4)
_cell_length_b                   11.8008(6)
_cell_length_c                   13.0936(7)
_cell_measurement_reflns_used    3892
_cell_measurement_temperature    173
_cell_measurement_theta_max      70.8030
_cell_measurement_theta_min      4.4200
_cell_volume                     1294.63(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.44a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.44a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.44a (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_temperature      173.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.956
_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   -105.00 -19.00   1.00    4.93    --  -36.88 -38.00 -90.00   86
  2  \w    -95.00 -48.00   1.00    4.93    --  -36.88 144.00 -10.00   47
  3  \w    -32.00  56.00   1.00    4.93    --   36.88 -38.00   0.00   88
  4  \w     11.00 101.00   1.00    4.93    --   36.88-144.00 -63.00   90
  5  \w     18.00 104.00   1.00    4.93    --   36.88  38.00-180.00   86
  6  \w     40.00 118.00   1.00   17.00    --  107.00 -45.00-150.00   78
  7  \w     43.00 135.00   1.00   17.00    --  107.00 -91.00 129.29   92
  8  \w    101.00 174.00   1.00   17.00    --  107.00  61.00 -90.00   73
  9  \w     39.00 124.00   1.00   17.00    --  107.00 -45.00 120.00   85
 10  \w     39.00 114.00   1.00   17.00    --  107.00 -45.00   0.00   75
 11  \w     64.00 121.00   1.00   17.00    --  107.00 -45.00 -90.00   57
 12  \w     39.00 176.00   1.00   17.00    --  107.00   0.00-120.00  137
 13  \w     59.00 143.00   1.00   17.00    --  107.00 -93.00 -31.64   84
 14  \w     86.00 125.00   1.00   17.00    --  107.00 -93.00-161.34   39
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0420351000
_diffrn_orient_matrix_UB_12      -0.0347276000
_diffrn_orient_matrix_UB_13      0.1008066000
_diffrn_orient_matrix_UB_21      0.0239613000
_diffrn_orient_matrix_UB_22      -0.1230789000
_diffrn_orient_matrix_UB_23      -0.0748591000
_diffrn_orient_matrix_UB_31      0.1674771000
_diffrn_orient_matrix_UB_32      0.0608886000
_diffrn_orient_matrix_UB_33      0.0064016000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6991
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.071
_diffrn_reflns_theta_min         5.005
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.980
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.44a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.062
_exptl_crystal_description       block
_exptl_crystal_F_000             430
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0012(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         4792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0798
_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^)+(0.0461P)^2^+7.2340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4249
_reflns_number_total             4792
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03084_si_002.cif
_cod_data_source_block           9
_cod_database_code               4345813
_shelxl_version_number           2014-1
_chemical_oxdiff_formula         ZnC50H50N14F6S2O10
_reflns_odcompleteness_completeness 98.19
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C19(H19), C16(H16), C18(H18), C2(H2), C17(H17), C5(H5), C9(H9), C3(H3),
 C10(H10), C12(H12), C11(H11), C4(H4)
2.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              19242
_shelx_hkl_checksum              67988
_shelx_fab_checksum              86641
_olex2_date_sample_data_collection 2017-02-13
_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 1.205
_oxdiff_exptl_absorpt_empirical_full_min 0.626