Copper (ii) dimers stabilized by bis(phenol) amine ligands: theoretical and experimental insights
Rajput, Amit; Kumar, Akhilesh; Sengupta, Arunava; Tyagi, Priyanka; Arora, Himanshu; New Journal of Chemistry 42 (2018) 12621–; doi:10.1039/C8NJ02591F

data_7057518
_publ_section_title
;
 Copper (ii) dimers stabilized by bis(phenol) amine ligands: theoretical
 and experimental insights
;
_journal_issue                   15
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12621
_journal_paper_doi               10.1039/C8NJ02591F
_journal_volume                  42
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C68 H102 Cu2 N2 O8'
_chemical_formula_sum            'C68 H102 Cu2 N2 O8'
_chemical_formula_weight         1202.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-06 deposited with the CCDC.
2018-06-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2578(17)
_cell_length_b                   15.878(2)
_cell_length_c                   37.239(6)
_cell_measurement_reflns_used    10548
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.31
_cell_measurement_theta_min      1.9
_cell_volume                     6656.5(17)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'Bruker SMART APEX'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.1025
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            38265
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.890
_diffrn_source                   'fine focused sealed tube'
_exptl_absorpt_coefficient_mu    0.691
_exptl_absorpt_correction_T_max  0.9341
_exptl_absorpt_correction_T_min  0.8741
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   0.934
_exptl_transmission_factor_min   0.871
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 3688 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     721
_refine_ls_number_reflns         13475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0549
_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^)+(0.0529P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1257
_reflns_Friedel_coverage         0.798
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                10548
_reflns_number_total             13475
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj02591f2.cif
_cod_data_source_block           4octem
_cod_depositor_comments
'Adding full bibliography for 7057517--7057518.cif.'
_cod_original_cell_volume        6656.6(17)
_cod_database_code               7057518
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.871
_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.a Ternary CH refined with riding coordinates:
 C31(H31), C65(H65)
2.b Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C16(H16A,H16B), C49(H49A,H49B), C50(H50A,H50B)
2.c Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,
 H29B,H29C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C38(H38A,H38B,H38C),
 C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C44(H44A,H44B,H44C), C45(H45A,H45B,
 H45C), C46(H46A,H46B,H46C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,
 H57B,H57C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C),
 C66(H66A,H66B,H66C), C68(H68A,H68B,H68C)
2.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C18(H18), C24(H24), C41(H41), C47(H47), C52(H52), C58(H58)
;
_shelx_res_checksum              51745
_olex2_submission_special_instructions 'No special instructions were received'