Synthesis and structural, redox and photophysical properties of tris-(2,5-di(2-pyridyl)pyrrolide) lanthanide complexes.
McPherson, James N.; Abad Galan, Laura; Iranmanesh, Hasti; Massi, Massimiliano; Colbran, Stephen B.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 9365–9375; doi:10.1039/c9dt01262a

data_7700169
_publ_section_title
;
 Synthesis and structural, redox and photophysical properties of
 tris-(2,5-di(2-pyridyl)pyrrolide) lanthanide complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9365
_journal_page_last               9375
_journal_paper_doi               10.1039/c9dt01262a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '2(C51 H42 Eu N9 O6), H2 O'
_chemical_formula_sum            'C102 H86 Eu2 N18 O13'
_chemical_formula_weight         2075.80
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-24 deposited with the CCDC.    2019-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.717(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.3254(12)
_cell_length_b                   13.3245(9)
_cell_length_c                   19.4895(13)
_cell_measurement_reflns_used    9897
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.98
_cell_measurement_theta_min      2.59
_cell_volume                     4498.8(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       '<i>APEX3 </i>(Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      99.95
_diffrn_detector_type            'Photon II detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 Quest'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1555
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            146595
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.200
_diffrn_source                   'Incoated I\mS 3.0 Microfocus source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.458
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       plate
_exptl_crystal_F_000             2108
_exptl_crystal_preparation       Luminescent
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         7935
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0486P)^2^+13.5680P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5611
_reflns_number_total             7935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01262a2.cif
_cod_data_source_block           james_eu_june18_0m_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7700168--7700170.cif.
;
_cod_database_code               7700169
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O1C-C8C = O1C'-C8C'
 1.2 with sigma of 0.02
 O2C'-C8C' = O2C-C8C
 1.35 with sigma of 0.02
 C9C'-O2C' = C9C-O2C
 1.47 with sigma of 0.02
 C8C'-C9C'
 2.36 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C8C') = Uanis(C8C)
4. Rigid body (RIGU) restrains
 C8C, O1C, O2C, C9C, C9C', O2C', C8C', O1C'
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: O2C'(0.4) C8C(0.6) C8C'(0.4) O1C'(0.4) C9C'(0.4) H9CA(0.4)
 H9CB(0.4) H9CC(0.4) O1(0.5) H1D(0.5) H1E(0.5) O2C(0.6) O1C(0.6) C9C(0.6)
 H9CD(0.6) H9CE(0.6) H9CF(0.6)
6.a Free rotating group:
 O1(H1D,H1E)
6.b Aromatic/amide H refined with riding coordinates:
 C1A(H1A), C17B(H17B), C14A(H14A), C17A(H17A), C4A(H4A), C2A(H2A), C1C(H1C),
 C4C(H4C), C2C(H2C), C16B(H16B), C17C(H17C), C14B(H14B), C15A(H15A), C1B(H1B),
 C3C(H3C), C16A(H16A), C15C(H15C), C14C(H14C), C16C(H16C), C15B(H15B), C3A(H3A),
  C4B(H4B), C2B(H2B), C3B(H3B)
6.c Idealised Me refined with riding coordinates:
 C9C(H9CD,H9CE,H9CF)
6.d Idealised Me refined as rotating group:
 C11B(H11A,H11B,H11C), C11C(H11D,H11E,H11F), C11A(H11G,H11H,H11I), C9B(H9BA,
 H9BB,H9BC), C9A(H9AA,H9AB,H9AC), C9C'(H9CA,H9CB,H9CC)
;
_shelx_res_checksum              5910
_olex2_submission_special_instructions 'No special instructions were received'