Combinatorial Synthesis of Acacen-Type Ligands and Their Coordination Compounds.
Tomažin, Urša; Grošelj, Uroš; Počkaj, Marta; Požgan, Franc; Štefane, Bogdan; Svete, Jurij; ACS combinatorial science 19 (2017) 386–396; doi:10.1021/acscombsci.7b00027

data_4514157
_publ_section_title
;
 Combinatorial Synthesis of Acacen-Type Ligands and Their Coordination
 Compounds.
;
_journal_issue                   6
_journal_name_full               'ACS combinatorial science'
_journal_page_first              386
_journal_page_last               396
_journal_paper_doi               10.1021/acscombsci.7b00027
_journal_volume                  19
_journal_year                    2017
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C28 H34 Cu N2 O2'
_chemical_formula_sum            'C28 H34 Cu N2 O2'
_chemical_formula_weight         494.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 93.9320(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4654(2)
_cell_length_b                   14.3184(3)
_cell_length_c                   14.1523(3)
_cell_measurement_reflns_used    5961
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2520.02(9)
_computing_cell_refinement       'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 2000)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_unetI/netI     0.0332
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37594
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.85
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.8
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinovski& Minor, 1997)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.699
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.321
_refine_ls_abs_structure_details
;
 Flack x determined using 3960 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.014(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.161
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     606
_refine_ls_number_reflns         11311
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.161
_refine_ls_R_factor_all          0.0719
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1162P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1307
_refine_ls_wR_factor_ref         0.1711
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    0.975
_reflns_Friedel_fraction_max     0.962
_reflns_number_gt                9715
_reflns_number_total             11311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            co7b00027_si_005.cif
_cod_data_source_block           shelx
_cod_database_code               4514157
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              87645
_shelx_hkl_checksum              94081