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_4345810
_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         'C80 H64 Br2 Cu2 N24, Br6 Cu2, 4(C2 H3 N)'
_chemical_formula_sum            'C88 H76 Br8 Cu4 N28'
_chemical_formula_weight         2419.20
_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   geom
_audit_creation_date             2016-02-23
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 122.782(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.215(2)
_cell_length_b                   13.4835(10)
_cell_length_c                   25.8172(18)
_cell_measurement_reflns_used    29234
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.4
_cell_volume                     9428.2(12)
_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      100.0
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type
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Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1882
_diffrn_reflns_av_unetI/netI     0.1905
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            9519
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_min         2.441
_exptl_absorpt_coefficient_mu    4.341
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.180
_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            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       plate
_exptl_crystal_F_000             4784
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.705
_refine_diff_density_min         -1.114
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         9519
_refine_ls_number_restraints     68
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.2346
_refine_ls_R_factor_gt           0.1409
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3466
_refine_ls_wR_factor_ref         0.3856
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4467
_reflns_number_total             9519
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b03084_si_002.cif
_cod_data_source_block           EL294B
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        9428.1(12)
_cod_database_code               4345810
_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. Restrained distances
 N13-C41
 1.1 with sigma of 0.02
 N14-C43
 1.1 with sigma of 0.02
 C41-C42
 1.53 with sigma of 0.02
 C43-C44
 1.53 with sigma of 0.02
3. Rigid bond restraints
 C21, C22
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N13, C41, C42
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C21) \\sim Ueq, Uanis(C22) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(N13) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of
0.1 and sigma for terminal atoms of 0.2
Uanis(C43) \\sim Ueq, Uanis(N14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.1
Uanis(C21) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.1
5. Rigid body (RIGU) restrains
 C21, C22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N13, C41, C42
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C14(H14A,H14B), C27(H27A,H27B), C34(H34A,H34B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12),
 C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
  C30(H30), C31(H31), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39), C40(H40)
6.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C42(H42A,H42B,H42C)
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_shelx_res_checksum              66737
_shelx_hkl_checksum              75917
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'