Excitation modulation of Eu:BPEPC based complexes as low-energy reference standards for circularly polarised luminescence (CPL).
starck, matthieu; MacKenzie, Lewis Edward; Batsanov, Andrei Stepanovich; Parker, David; Pal, Robert; Chemical Communications  (2019) –; doi:10.1039/C9CC07290J

data_7124418
_publ_section_title
;
 Excitation modulation of Eu:BPEPC based complexes as low-energy reference
 standards for circularly polarised luminescence (CPL).
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07290J
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C96 H87 Eu N9 O9 3+, 3(Cl 1-), C5 H12 O, 4.5(C H4 O), 0.5(H2 O)'
_chemical_formula_sum            'C105.5 H118 Cl3 Eu N9 O15'
_chemical_formula_weight         2010.39
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-22
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.08.16 svn.r3652 for OlexSys, GUI svn.r5895)
;
_audit_update_record
;
2019-09-10 deposited with the CCDC.	2019-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.7747(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.9608(11)
_cell_length_b                   23.1000(12)
_cell_length_c                   22.9095(13)
_cell_measurement_reflns_used    9275
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.69
_cell_measurement_theta_min      2.32
_cell_volume                     10341.2(10)
_computing_cell_refinement       'SAINT v8.38A (Bruker, 2017)'
_computing_data_collection       'APEX3 v.2016.1-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT v8.38A (Bruker, 2017)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL 2018/3 multi-CPU (Sheldrick, 2015a)'
_computing_structure_solution    'ShelXT 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '3-circle area detector diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'focusing mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0582
_diffrn_reflns_av_unetI/netI     0.0711
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            233259
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.168
_diffrn_reflns_theta_min         2.048
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\mS microsource'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.9799
_exptl_absorpt_correction_T_min  0.8313
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 SADABS-2016/2 (Krause et al., 2015) was used for absorption correction. 
  wR2(int) was 0.1445 before and 0.0466 after correction. The Ratio 
  of minimum to maximum transmission is 0.8484. The \l/2 correction 
  factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       prism
_exptl_crystal_F_000             4192
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH, MeOBu-t'
_exptl_crystal_size_max          0.431
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.610
_refine_diff_density_min         -0.496
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details
;
 Flack x determined using 20334 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons et al., 2013). 
 x = -0.021(4) by classical fit to all intensities. 
 Hooft parameter y = -0.0113(14).
;
_refine_ls_abs_structure_Flack   -0.0231(15)
_refine_ls_extinction_coef       0.00016(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick, 2015a)'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2559
_refine_ls_number_reflns         60952
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0396P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.952
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                49312
_reflns_number_total             60952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc07290j2.cif
_cod_data_source_block           Eu(RR-L)3Cl3_19s028
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7124418
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.738
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups, All O(H,H)
  groups
2. Restrained distances
 C18S-C18T = C18T-O10T = O10S-C18S
 1.4 with sigma of 0.01
 C89B-C88B \\sim C89-C88
 with sigma of 0.02
 C95-C90 \\sim C91-C90
 with sigma of 0.02
 O9T-C17S \\sim O9S-C17S
 with sigma of 0.02
 O11T-C19S \\sim O11S-C19S
 with sigma of 0.02
 O11S-C19S \\sim O11T-C19S
 with sigma of 0.02
 C92-C91 \\sim C95-C94
 with sigma of 0.02
 C93-C92 \\sim C94-C93
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C88B \\sim C88: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C42B \\sim C42: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O11T \\sim O11S: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C18T \\sim C18S: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C89 \\sim C89B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
O12S \\sim O12T: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Cl3 \\sim Cl3B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C94 \\sim C94B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C95 \\sim C95B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C90 \\sim C90B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C91 \\sim C91B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C92 \\sim C92B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C91' \\sim C91D: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C92' \\sim C92D: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
Uanis(C93) = Uanis(C93B)
Uanis(C42B) = Uanis(C42)
Uiso(C89B) = Uiso(C89)
Uanis(C22') = Uanis(C21D)
Uanis(C90') = Uanis(C90D)
Uiso(C88B) = Uiso(C88)
4. Others
 Fixed Sof: H9B(0.4) H9A(0.6) O8(0.75) C42(0.75) C43(0.75) H43(0.75) C44(0.75)
 H44(0.75) C45(0.75) C46(0.75) H46(0.75) C47(0.75) H47(0.75) C64(0.75)
 H64A(0.75) H64B(0.75) H64C(0.75) C88(0.6) H88(0.6) C89(0.6) H89A(0.6)
 H89B(0.6) H89C(0.6) C90(0.6) C91(0.6) H91(0.6) C92(0.6) H92(0.6) C93(0.6)
 H93(0.6) C94(0.6) H94(0.6) C95(0.6) H95(0.6) O8B(0.25) C45B(0.25) C44B(0.25)
 H44B(0.25) C43B(0.25) H43B(0.25) C42B(0.25) C47B(0.25) H47B(0.25) C46B(0.25)
 H46B(0.25) C64B(0.25) H64D(0.25) H64E(0.25) H64F(0.25) C88B(0.4) H88B(0.4)
 C89B(0.4) H89D(0.4) H89E(0.4) H89F(0.4) C90B(0.4) C95B(0.4) H95B(0.4)
 C94B(0.4) H94B(0.4) C93B(0.4) H93B(0.4) C92B(0.4) H92B(0.4) C91B(0.4)
 H91B(0.4) C18'(0.85) C19'(0.85) H19'(0.85) C20'(0.85) H20'(0.85) C21'(0.85)
 H21'(0.85) C22'(0.85) H22'(0.85) C23'(0.85) H23'(0.85) C90'(0.85) C91'(0.85)
 H91'(0.85) C92'(0.85) H92'(0.85) C93'(0.85) H93'(0.85) C94'(0.85) H94'(0.85)
 C95'(0.85) H95'(0.85) C18D(0.15) C23D(0.15) H23D(0.15) C22D(0.15) H22D(0.15)
 C21D(0.15) H21D(0.15) C20D(0.15) H20D(0.15) C19D(0.15) H19D(0.15) C90D(0.15)
 C95D(0.15) H95D(0.15) C94D(0.15) H94D(0.15) C93D(0.15) H93D(0.15) C92D(0.15)
 H92D(0.15) C91D(0.15) H91D(0.15) H19A(0.6) H19B(0.6) H19C(0.6) H19E(0.4)
 H19F(0.4) H19G(0.4) O11S(0.6) H11S(0.6) O11T(0.4) H11T(0.4) O9S(0.7) H9S(0.7)
 H17G(0.7) H17H(0.7) H17I(0.7) H17J(0.3) H17K(0.3) H17L(0.3) O10S(0.6)
 H10S(0.6) C18S(0.6) H18A(0.6) H18B(0.6) H18C(0.6) O10T(0.4) H10T(0.4)
 C18T(0.4) H18D(0.4) H18E(0.4) H18F(0.4) O12T(0.3) H12D(0.3) H12E(0.3)
 O12S(0.7) H12F(0.7) H12G(0.7) Cl3(0.6) Cl3B(0.4) O9T(0.3) H9T(0.3)
5.a Riding coordinates:
 C88(H88), C89(H89A,H89B,H89C), C9S(H9SA,H9SB,H9SC), C19S(H19A,H19B,H19C),
 C19S(H19E,H19F,H19G), O11S(H11S), O11T(H11T), O9S(H9S), C17S(H17G,H17H,H17I),
 C17S(H17J,H17K,H17L), C16S(H16A,H16B,H16C), O3S(H3S), C11S(H11A,H11B,H11C),
 O4S(H4S), O10S(H10S), C18S(H18A,H18B,H18C), O10T(H10T), C18T(H18D,H18E,H18F),
 O12T(H12D,H12E), O12S(H12F,H12G), O9T(H9T)
5.b Rotating group:
 C64(H64A,H64B,H64C)
5.c Ternary CH refined with riding coordinates:
 C16(H16), C24(H24), C48(H48), C56(H56), C80(H80), C88B(H88B), C16'(H16'),
 C24'(H24'), C48'(H48'), C56'(H56'), C80'(H80'), C88'(H88')
5.d Me refined with riding coordinates:
 C64B(H64D,H64E,H64F), C89B(H89D,H89E,H89F)
5.e Aromatic/amide H refined with riding coordinates:
 N4(H4), N5(H5), N6(H6), N7(H7), N8(H8), N9(H9B), N9(H9A), C3(H3), C5(H5A),
 C11(H11), C12(H12), C14(H14), C15(H15), C19(H19), C20(H20), C21(H21), C22(H22),
  C23(H23), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C35(H35),
 C37(H37), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C59(H59), C60(H60),
  C61(H61), C62(H62), C63(H63), C67(H67), C69(H69), C75(H75), C76(H76),
 C78(H78), C79(H79), C83(H83), C84(H84), C85(H85), C86(H86), C87(H87), C43(H43),
  C44(H44), C46(H46), C47(H47), C91(H91), C92(H92), C93(H93), C94(H94),
 C95(H95), C44B(H44B), C43B(H43B), C47B(H47B), C46B(H46B), C95B(H95B),
 C94B(H94B), C93B(H93B), C92B(H92B), C91B(H91B), N4'(H4'), N5'(H5'), N6'(H6'),
 N7'(H7'), N8'(H8'), N9'(H9'), C3'(H3'), C5'(H5'A), C11'(H11'), C12'(H12'),
 C14'(H14'), C15'(H15'), C27'(H27'), C28'(H28'), C29'(H29'), C30'(H30'),
 C31'(H31'), C35'(H35'), C37'(H37'), C43'(H43'), C44'(H44'), C46'(H46'),
 C47'(H47'), C51'(H51'), C52'(H52'), C53'(H53'), C54'(H54'), C55'(H55'),
 C59'(H59'), C60'(H60'), C61'(H61'), C62'(H62'), C63'(H63'), C67'(H67'),
 C69'(H69'), C75'(H75'), C76'(H76'), C78'(H78'), C79'(H79'), C83'(H83'),
 C84'(H84'), C85'(H85'), C86'(H86'), C87'(H87'), C19'(H19'), C20'(H20'),
 C21'(H21'), C22'(H22'), C23'(H23'), C91'(H91'), C92'(H92'), C93'(H93'),
 C94'(H94'), C95'(H95'), C23D(H23D), C22D(H22D), C21D(H21D), C20D(H20D),
 C19D(H19D), C95D(H95D), C94D(H94D), C93D(H93D), C92D(H92D), C91D(H91D)
5.f Fitted hexagon refined as free rotating group:
 C45B(C44B,C43B,C42B,C47B,C46B), C90B(C95B,C94B,C93B,C92B,C91B), C18D(C23D,
 C22D,C21D,C20D,C19D), C90D(C95D,C94D,C93D,C92D,C91D)
5.g Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C32(H32A,H32B,H32C), C49(H49A,H49B,
 H49C), C57(H57A,H57B,H57C), C81(H81A,H81B,H81C), C96(H96A,H96B,H96C),
 C17'(H17D,H17E,H17F), C25'(H25D,H25E,H25F), C32'(H32D,H32E,H32F), C49'(H49D,
 H49E,H49F), C57'(H57D,H57E,H57F), C64'(H64G,H64H,H64I), C81'(H81D,H81E,H81F),
 C89'(H89G,H89H,H89I), C96'(H96D,H96E,H96F), C1S(H1SA,H1SB,H1SC), C3S(H3SA,H3SB,
 H3SC), C4S(H4SA,H4SB,H4SC), C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,H6SC), C8S(H8SA,
 H8SB,H8SC), C10S(H10A,H10B,H10C), C14S(H14A,H14B,H14C), C15S(H15A,H15B,H15C),
 C12S(H12A,H12B,H12C), C13S(H13A,H13B,H13C)
5.h Idealised tetrahedral OH refined as rotating group:
 O6S(H6S), O7S(H7S), O8S(H8S), O5S(H5S)
;
_shelx_res_checksum              68023
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'