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_4345814
_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         'C88 H84 Cu2 N24 O2, 4(C F3 O3 S), 4(C3 H6 O)'
_chemical_formula_sum            'C104 H108 Cu2 F12 N24 O18 S4'
_chemical_formula_weight         2465.46
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                90
_cell_angle_beta                 110.418(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.7957(11)
_cell_length_b                   22.4426(10)
_cell_length_c                   27.7251(19)
_cell_measurement_reflns_used    12013
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.3130
_cell_measurement_theta_min      2.3140
_cell_volume                     12709.7(13)
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type
;
Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC12 goniometer and HG Saturn 724+ detector
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1674
_diffrn_reflns_av_unetI/netI     0.1259
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            62999
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_min         2.062
_exptl_absorpt_coefficient_mu    0.485
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_description       block
_exptl_crystal_F_000             5096
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.973
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         11194
_refine_ls_number_restraints     112
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.1926
_refine_ls_R_factor_gt           0.0986
_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^)+(0.1712P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2552
_refine_ls_wR_factor_ref         0.3142
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4836
_reflns_number_total             11194
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03084_si_002.cif
_cod_data_source_block           10
_cod_database_code               4345814
_shelxl_version_number           2014-1
_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, All O(H,H) groups
2. Rigid bond restraints
 C46, S2, O5, O6, O7, F5, F6, F4, S2, O5, S2, O6, S2, O7, S2, C46, F5, C46, F6,
  C46, F4, C46
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
F5 \\sim S2 \\sim O5 \\sim O6 \\sim O7 \\sim C46 \\sim F6 \\sim F4 \\sim S2
\\sim O5 \\sim S2 \\sim O6 \\sim S2 \\sim O7 \\sim S2 \\sim C46 \\sim F5 \\sim
C46 \\sim F6 \\sim C46 \\sim F4 \\sim C46: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 F5, S2, O5, O6, O7, C46, F6, F4, S2, O5, S2, O6, S2, O7, S2, C46, F5, C46, F6,
  C46, F4, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Rotating group:
 O1(H1A,H1B)
5.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C8(H8A,H8B), C37(H37A,H37B), C30(H30A,H30B)
5.c Me refined with riding coordinates:
 C50(H50A,H50B,H50C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C52(H52A,H52B,
 H52C), C21(H21A,H21B,H21C), C5(H5A,H5B,H5C), C27(H27A,H27B,H27C), C41(H41A,
 H41B,H41C)
5.d Aromatic/amide H refined with riding coordinates:
 C35(H35), C32(H32), C33(H33), C13(H13), C3(H3), C10(H10), C11(H11), C22(H22),
 C18(H18), C12(H12), C7(H7), C6(H6), C34(H34), C28(H28), C43(H43), C24(H24),
 C25(H25), C39(H39), C42(H42), C19(H19)
;
_shelx_res_checksum              6100
_shelx_hkl_checksum              72366
_shelx_fab_checksum              81490
_olex2_submission_special_instructions 'No special instructions were received'