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_4349015
_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         'C48 H46 N6 O6 Zn2, C H4 O'
_chemical_formula_sum            'C49 H50 N6 O7 Zn2'
_chemical_formula_weight         965.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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
;
2015-10-09 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                87.20(3)
_cell_angle_beta                 88.48(3)
_cell_angle_gamma                89.90(3)
_cell_formula_units_Z            4
_cell_length_a                   12.804(3)
_cell_length_b                   17.462(3)
_cell_length_c                   19.515(4)
_cell_measurement_temperature    100(2)
_cell_volume                     4356.5(16)
_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 0.897
_diffrn_measured_fraction_theta_max 0.885
_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  0.0488
_diffrn_reflns_av_unetI/netI     0.0407
_diffrn_reflns_Laue_measured_fraction_full 0.897
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            85475
_diffrn_reflns_point_group_measured_fraction_full 0.897
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.069
_diffrn_reflns_theta_min         1.045
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    1.162
_exptl_crystal_colour            grey
_exptl_crystal_density_diffrn    1.472
_exptl_crystal_description       prism
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.568
_refine_diff_density_min         -0.976
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1161
_refine_ls_number_reflns         22649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0902P)^2^+11.5914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1704
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19771
_reflns_number_total             22649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00200a2.cif
_cod_data_source_block           p-1
_cod_original_cell_volume        4356.5(15)
_cod_database_code               4349015
_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
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14A(H14A,H14B), C15A(H15A,H15B), C16A(H16A,H16B), C17A(H17A,H17B), C18A(H18A,
 H18B), C19A(H19A,H19B), C14B(H14C,H14D), C15B(H15C,H15D), C16B(H16C,H16D),
 C17B(H17C,H17D), C18B(H18C,H18D), C19B(H19C,H19D), C14C(H14E,H14F), C15C(H15E,
 H15F), C16C(H16E,H16F), C17C(H17E,H17F), C18C(H18E,H18F), C19C(H19E,H19F),
 C14D(H14G,H14H), C15D(H15G,H15H), C16D(H16G,H16H), C17D(H17G,H17H), C18D(H18G,
 H18H), C19D(H19G,H19H)
2.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C2A(H2A), C3A(H3A), C5A(H5A), C6A(H6A), C7A(H7A), C10A(H10A),
 C12A(H12A), C1B(H1B), C2B(H2B), C3B(H3B), C5B(H5B), C6B(H6B), C7B(H7B),
 C10B(H10B), C12B(H12B), C1C(H1C), C2C(H2C), C3C(H3C), C5C(H5C), C6C(H6C),
 C7C(H7C), C10C(H10C), C12C(H12C), C1D(H1D), C2D(H2D), C3D(H3D), C5D(H5D),
 C6D(H6D), C7D(H7D), C10D(H10D), C12D(H12D)
2.c Idealised Me refined as rotating group:
 C2AA(H2AA,H2AB,H2AC), C2BB(H2BA,H2BB,H2BC), C2CC(H2CA,H2CB,H2CC), C2DD(H2DA,
 H2DB,H2DC), C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC)
2.d Idealised tetrahedral OH refined as rotating group:
 O1S(H1S), O2S(H2S)
;
_shelx_res_checksum              2565
_shelx_hkl_checksum              61564
_olex2_submission_special_instructions 'No special instructions were received'