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_4349012
_publ_section_title
;
 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         'C49 H49 Mn2 N6 O8, C H4 O'
_chemical_formula_sum            'C50 H53 Mn2 N6 O9'
_chemical_formula_weight         991.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                90
_cell_angle_beta                 94.73(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.460(2)
_cell_length_b                   12.325(2)
_cell_length_c                   18.253(4)
_cell_measurement_temperature    100(2)
_cell_volume                     2345.2(8)
_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 0.992
_diffrn_measured_fraction_theta_max 0.985
_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  0.1022
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            45777
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.164
_diffrn_reflns_theta_min         2.239
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    0.602
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       prism
_exptl_crystal_F_000             1034
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.733
_refine_diff_density_min         -0.779
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         6854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0804
_refine_ls_R_factor_gt           0.0638
_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^)+(0.0952P)^2^+3.7876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1797
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5478
_reflns_number_total             6854
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00200a2.cif
_cod_data_source_block           p21byn
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4349012
_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. Others
 Fixed Sof: C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) O5(0.5) H5A(0.5) C26(0.5)
 H26A(0.5) H26B(0.5) H26C(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)
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)
3.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
3.d Idealised tetrahedral OH refined as rotating group:
 O5(H5A)
;
_shelx_res_checksum              7420
_shelx_hkl_checksum              51408
_olex2_submission_special_instructions 'No special instructions were received'