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_4345808
_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         '2(C20 H16 Cl2 Cu N6)'
_chemical_formula_sum            'C40 H32 Cl4 Cu2 N12'
_chemical_formula_weight         949.65
_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     direct
_audit_creation_date             2016-09-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.08.25 svn.r3337 for OlexSys, GUI svn.r5221)
;
_cell_angle_alpha                97.491(5)
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_cell_formula_units_Z            2
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_cell_length_b                   13.9067(7)
_cell_length_c                   14.9267(10)
_cell_measurement_reflns_used    3811
_cell_measurement_temperature    173
_cell_measurement_theta_max      71.2210
_cell_measurement_theta_min      5.4080
_cell_volume                     1888.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
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_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 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
  1 omega   39.00   77.00   1.0000   12.5000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  -90.0000 38

  2 omega  -58.00  -33.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000   90.0000 25

  3 omega -100.00   -5.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  105.0000 -125.0000 95

  4 omega -118.00  -92.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  -57.0000   90.0000 26

  5 omega   29.00  123.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   38.0000 -150.0000 94

  6 omega   29.00  123.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500   77.0000   90.0000 94

  7 omega   -8.00   82.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -77.0000  -30.0000 90

  8 omega   39.00   69.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  -90.0000 30

  9 omega   37.00   62.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -150.0000 25

 10 omega   41.00   70.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  -30.0000 29

 11 omega   45.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000   60.0000 26

 12 omega   39.00   66.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000   30.0000 27

 13 omega   41.00   70.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  -60.0000 29

 14 omega   42.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000   90.0000 29

 15 omega   38.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000    0.0000 33

 16 omega   45.00  136.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000   90.0000 91

 17 omega   37.00   67.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000 -120.0000 30

 18 omega   42.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  150.0000 29

 19 omega   41.00  103.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000 -120.0000 62

 20 omega  123.00  148.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000 -120.0000 25

 21 omega   91.00  117.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   64.0000   30.0000 26

 22 omega  133.00  177.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000   64.0000   30.0000 44

 23 omega   41.00   71.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  120.0000 30

 24 omega   41.00  147.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000  -60.0000 106

 25 omega   41.00  176.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      109.5000    0.0000 -150.0000 135
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0776676000
_diffrn_orient_matrix_UB_12      -0.0032279000
_diffrn_orient_matrix_UB_13      -0.1039729000
_diffrn_orient_matrix_UB_21      0.1220776000
_diffrn_orient_matrix_UB_22      0.0775810000
_diffrn_orient_matrix_UB_23      -0.0079981000
_diffrn_orient_matrix_UB_31      0.0852454000
_diffrn_orient_matrix_UB_32      -0.0819739000
_diffrn_orient_matrix_UB_33      -0.0275865000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0925
_diffrn_reflns_av_unetI/netI     0.1085
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10662
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        66.995
_diffrn_reflns_theta_max         66.995
_diffrn_reflns_theta_min         4.821
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.406
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.30584
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             964
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.883
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         6539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0890P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1603
_refine_ls_wR_factor_ref         0.1878
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4540
_reflns_number_total             6539
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03084_si_002.cif
_cod_data_source_block           el415c
_cod_database_code               4345808
_chemical_oxdiff_formula         C60H60O20Co2
_reflns_odcompleteness_completeness 98.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C34(H34A,H34B), C27(H27A,H27B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C5(H5), C39(H39), C17(H17), C2(H2), C25(H25), C36(H36), C12(H12),
 C31(H31), C32(H32), C20(H20), C9(H9), C4(H4), C23(H23), C11(H11), C3(H3),
 C18(H18), C19(H19), C30(H30), C29(H29), C38(H38), C24(H24), C37(H37), C10(H10)
;
_shelx_res_checksum              48916
_shelx_hkl_checksum              70318
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'