3d transition metal complexes with a julolidine‒quinoline based ligand: structures, spectroscopy and optical properties
Fanna, Daniel J.; Zhang, Yingjie; Li, Li; Karatchevtseva, Inna; Shepherd, Nicholas D.; Azim, Abdul; Price, Jason R.; Aldrich-Wright, Janice; Reynolds, Jason K.; Li, Feng; Inorganic Chemistry Frontiers 3 (2016) 286–; doi:10.1039/C5QI00200A

data_4349014
_publ_section_title
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 3d transition metal complexes with a julolidine--quinoline based ligand:
 structures, spectroscopy and optical properties
;
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              286
_journal_paper_doi               10.1039/C5QI00200A
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         '3(C24 H23 Cu N3 O3), C H4 O'
_chemical_formula_sum            'C73 H73 Cu3 N9 O10'
_chemical_formula_weight         1427.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.21 svn.r3230 for OlexSys, GUI svn.r5103)
;
_audit_update_record
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2015-10-09 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.29(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.9270(18)
_cell_length_b                   23.859(5)
_cell_length_c                   29.072(6)
_cell_measurement_temperature    100(2)
_cell_volume                     6127(2)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'ADSC Quantum Detector'
_diffrn_measurement_method       '\p  scans'
_diffrn_radiation_type
'silicon double crystal monochromated synchrotron'
_diffrn_radiation_wavelength     0.71074
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            124197
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.074
_diffrn_reflns_theta_min         1.109
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    1.105
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       prism
_exptl_crystal_F_000             2964
_exptl_crystal_size_max          0.020
_exptl_crystal_size_mid          0.010
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.464
_refine_diff_density_min         -4.124
_refine_diff_density_rms         0.172
_refine_ls_extinction_coef       0.0026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         17920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0894
_refine_ls_R_factor_gt           0.0816
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1225P)^2^+24.7129P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2296
_refine_ls_wR_factor_ref         0.2350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15640
_reflns_number_total             17920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00200a2.cif
_cod_data_source_block           p2byc
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349014
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: H61C(0.5) H61D(0.5) H61A(0.5) H61B(0.5) C62A(0.5) H62A(0.5)
 H62B(0.5) C62B(0.5) H62C(0.5) H62D(0.5) H63C(0.5) H63D(0.5) H63A(0.5) H63B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,
 H18B), C19(H19A,H19B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
 C41(H41A,H41B), C42(H42A,H42B), C61(H61C,H61D), C61(H61A,H61B), C62A(H62A,
 H62B), C62B(H62C,H62D), C63(H63C,H63D), C63(H63A,H63B), C64(H64A,H64B),
 C65(H65A,H65B), C66(H66A,H66B), C70(H70A,H70B)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C7(H7), C10(H10), C12(H12), C25(H25),
 C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C34(H34), C36(H36), C48(H48),
  C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C57(H57), C59(H59)
3.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C47(H47A,H47B,H47C), C73(H73A,H73B,H73C), C1S(H1SA,H1SB,
 H1SC)
3.d Idealised tetrahedral OH refined as rotating group:
 O1S(H1S)
;
_shelx_res_checksum              20942
_shelx_hkl_checksum              86479
_olex2_submission_special_instructions 'No special instructions were received'