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_4345809
_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         'C40 H32 Cl10 Cu5 N12'
_chemical_formula_sum            'C40 H32 Cl10 Cu5 N12'
_chemical_formula_weight         1352.97
_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             2015-06-14
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                101.609(6)
_cell_angle_beta                 104.227(7)
_cell_angle_gamma                91.061(7)
_cell_formula_units_Z            1
_cell_length_a                   10.2604(8)
_cell_length_b                   10.5576(8)
_cell_length_c                   11.3368(8)
_cell_measurement_reflns_used    2765
_cell_measurement_temperature    173
_cell_measurement_theta_max      71.5130
_cell_measurement_theta_min      4.3160
_cell_volume                     1163.05(16)
_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
;
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)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1033
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
  1 omega   16.00  128.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -       54.7500   19.0000   30.0000 112

  2 omega   90.00  123.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -64.0000  120.0000 33

  3 omega   44.00   72.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000  150.0000 28

  4 omega   46.00   73.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -64.0000  120.0000 27

  5 omega   38.00   71.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000   90.0000 33

  6 omega   41.00   71.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000   30.0000 30

  7 omega   37.00   62.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000    0.0000 25

  8 omega   41.00   71.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  -60.0000 30

  9 omega   40.00   68.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000  -90.0000 28

 10 omega   39.00   66.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000  -90.0000 27

 11 omega   81.00  148.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000  -90.0000 67

 12 omega   69.00  148.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000 -180.0000 79

 13 omega   39.00  169.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -12.0000 -180.0000 130

 14 omega   91.00  165.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000   64.0000 -180.0000 74

 15 omega   77.00  126.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -       54.7500  125.0000 -150.0000 49

 16 omega   38.00   68.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -25.0000 -180.0000 30

 17 omega  -18.00   61.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -38.0000 -150.0000 79

 18 omega   42.00  146.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -92.0000   60.0000 104

 19 omega   40.00   71.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      109.5000  -38.0000   60.0000 31

 20 omega  -12.00   79.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -       54.7500  -77.0000  150.0000 91

 21 omega   17.00   42.00   1.0000    1.9100
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  120.0000 25

 22 omega  -24.00   12.00   1.0000    1.9100
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000  120.0000 36

 23 omega -104.00  -27.00   1.0000    7.6300
omega____ theta____ kappa____ phi______ frames
    -      -54.7500  125.0000  -30.0000 77
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1525845000
_diffrn_orient_matrix_UB_12      0.0153065000
_diffrn_orient_matrix_UB_13      -0.0402795000
_diffrn_orient_matrix_UB_21      0.0059626000
_diffrn_orient_matrix_UB_22      0.0816312000
_diffrn_orient_matrix_UB_23      0.1304197000
_diffrn_orient_matrix_UB_31      0.0282716000
_diffrn_orient_matrix_UB_32      0.1241269000
_diffrn_orient_matrix_UB_33      -0.0441513000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.979
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6774
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.499
_diffrn_reflns_theta_min         4.457
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.206
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82444
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_description       block
_exptl_crystal_F_000             671
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.706
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4317
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0520P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1040
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3494
_reflns_number_total             4317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03084_si_002.cif
_cod_data_source_block           el633
_cod_database_code               4345809
_chemical_oxdiff_formula         C50H50Cu2N10Cl2
_reflns_odcompleteness_completeness 98.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H3(0.035) H4(0.042) H5(0.037) H6(0.033) H7A(0.03) H7B(0.03)
 H10(0.035) H11(0.038) H12(0.038) H13(0.034) H14A(0.027) H14B(0.027) H17(0.031)
 H18(0.033) H19(0.039) H20(0.035)
 Fixed X: Cu3(1) H3(0.6262) H4(0.4358) H5(0.2211) H6(0.1875) H7A(0.7817)
 H7B(0.7878) H10(0.8189) H11(0.8948) H12(0.9312) H13(0.8656) H14A(0.8437)
 H14B(0.7009) H17(0.4342) H18(0.2527) H19(0.2706) H20(0.4686)
 Fixed Y: Cu3(0.5) H3(1.1736) H4(1.2901) H5(1.1875) H6(0.964) H7A(0.8231)
 H7B(0.9712) H10(0.8325) H11(1.0451) H12(1.1874) H13(1.1236) H14A(0.6674)
 H14B(0.6983) H17(0.4679) H18(0.5816) H19(0.7243) H20(0.7669)
 Fixed Z: Cu3(0.5) H3(0.8955) H4(0.8663) H5(0.7971) H6(0.7596) H7A(0.8982)
 H7B(0.9583) H10(0.4919) H11(0.5129) H12(0.7041) H13(0.865) H14A(0.689)
 H14B(0.709) H17(0.1791) H18(0.22) H19(0.4063) H20(0.5602)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'