#------------------------------------------------------------------------------
#$Date: 2017-12-03 20:15:53 +0200 (Sun, 03 Dec 2017) $
#$Revision: 203907 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/40/7044002.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7044002
loop_
_publ_author_name
'Craze, Alexander R.'
'Huang, Xin-Da'
'Etchells, Isaac'
'Zheng, Li-Min'
'Bhadbhade, Mohan'
'Marjo, Christopher'
'Clegg, Jack Kay'
'Moore, Evan G.'
'Avdeev, Maxim'
'Lindoy, Leonard F.'
'Li, Feng'
_publ_section_title
;
 Synthesis and Characterisation of New Tripodal Lanthanide Complexes and
 Investigation of Their Optical and Magnetic Properties
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02556D
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C39 H57 N7 O3'
_chemical_formula_sum            'C39 H57 N7 O3'
_chemical_formula_weight         671.93
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2017-08-18 deposited with the CCDC.
2017-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.6115(19)
_cell_length_b                   13.6115(19)
_cell_length_c                   35.291(7)
_cell_measurement_reflns_used    33332
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.81
_cell_measurement_theta_min      2.88
_cell_volume                     5662.5(16)
_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      100.15
_diffrn_measured_fraction_theta_full 0.9857
_diffrn_measured_fraction_theta_max 0.8499
_diffrn_measurement_device_type  'ADSC Q315r CCD area-detector'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       51
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            33332
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         31.81
_diffrn_reflns_theta_min         2.88
_diffrn_source                   'MX1 Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.076
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_density_diffrn    1.1822
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             2184.8532
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.005
_refine_diff_density_max         0.5053
_refine_diff_density_min         -0.3478
_refine_diff_density_rms         0.0549
_refine_ls_abs_structure_details
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.0(8)
_refine_ls_d_res_high            0.6741
_refine_ls_d_res_low             7.0635
_refine_ls_goodness_of_fit_ref   1.2796
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    28
_refine_ls_number_parameters     153
_refine_ls_number_reflns         3668
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.2794
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.0001
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1383
_reflns_Friedel_coverage         0.846
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              10
_reflns_limit_k_min              -10
_reflns_limit_l_max              51
_reflns_limit_l_min              -51
_reflns_number_gt                3564
_reflns_number_total             3668
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c7dt02556d2.cif
_cod_data_source_block           FL177_a
_cod_database_code               7044002
#BEGIN Tags that were not found in dictionaries:
_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
2. Restrained distances
 O1-H1
 0.87 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C2(H2a,H2b), C10(H10a,H10b), C12(H12a,H12b)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6), C9(H9), C8(H8)
3.c Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C13(H13a,H13b,H13c)
;
_olex2_submission_special_instructions 'No special instructions were received'
#END Tags that were not found in dictionaries
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -y,x-y,z
3 -x+y,-x,z
4 -x+y,y,z+1/2
5 x,x-y,z+1/2
6 -y,-x,z+1/2
7 x+1/3,y+2/3,z+2/3
8 -y+1/3,x-y+2/3,z+2/3
9 -x+y+1/3,-x+2/3,z+2/3
10 -x+y+1/3,y+2/3,z+7/6
11 x+1/3,x-y+2/3,z+7/6
12 -y+1/3,-x+2/3,z+7/6
13 x+2/3,y+1/3,z+1/3
14 -y+2/3,x-y+1/3,z+1/3
15 -x+y+2/3,-x+1/3,z+1/3
16 -x+y+2/3,y+1/3,z+5/6
17 x+2/3,x-y+1/3,z+5/6
18 -y+2/3,-x+1/3,z+5/6
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
O1 O 0.27676(8) 0.35995(7) 0.45616(2) 0.01866(18) Uani 1.000000 1 D . .
H1 H 0.318(2) 0.4155(16) 0.4406(6) 0.056(7) Uiso 1.000000 1 D . .
C1 C 0.37807(10) 0.59436(10) 0.35923(3) 0.0198(2) Uani 1.000000 1 . . .
H1a H 0.31534(10) 0.51477(10) 0.35787(3) 0.0237(3) Uiso 1.000000 1 R . .
H1b H 0.41022(10) 0.61772(10) 0.33347(3) 0.0237(3) Uiso 1.000000 1 R . .
N1 N 0.333333333333 0.666666666667 0.37186(4) 0.0163(3) Uani 1.000000 3 S T P
N2 N 0.41933(9) 0.53989(9) 0.42073(3) 0.0190(2) Uani 1.000000 1 . . .
C2 C 0.46985(11) 0.60150(11) 0.38593(3) 0.0213(2) Uani 1.000000 1 . . .
H2a H 0.51220(11) 0.56901(11) 0.37334(3) 0.0256(3) Uiso 1.000000 1 R . .
H2b H 0.52408(11) 0.68196(11) 0.39189(3) 0.0256(3) Uiso 1.000000 1 R . .
N3 N 0.28105(9) 0.35662(9) 0.59114(3) 0.0214(2) Uani 1.000000 1 . . .
C3 C 0.45094(10) 0.59186(10) 0.45256(4) 0.0189(2) Uani 1.000000 1 . . .
H3 H 0.50589(10) 0.67038(10) 0.45284(4) 0.0226(3) Uiso 1.000000 1 R . .
C5 C 0.31926(9) 0.41838(9) 0.48869(3) 0.0149(2) Uani 1.000000 1 . . .
C4 C 0.40487(10) 0.53369(10) 0.48809(3) 0.0167(2) Uani 1.000000 1 . . .
C6 C 0.27514(9) 0.36179(9) 0.52269(3) 0.0165(2) Uani 1.000000 1 . . .
H6 H 0.21492(9) 0.28531(9) 0.52228(3) 0.0198(2) Uiso 1.000000 1 R . .
C7 C 0.31811(10) 0.41584(10) 0.55772(3) 0.0171(2) Uani 1.000000 1 . . .
C9 C 0.44413(10) 0.58840(10) 0.52323(3) 0.0204(2) Uani 1.000000 1 . . .
H9 H 0.50058(10) 0.66642(10) 0.52357(3) 0.0244(3) Uiso 1.000000 1 R . .
C8 C 0.40326(10) 0.53234(10) 0.55725(3) 0.0198(2) Uani 1.000000 1 . . .
H8 H 0.43222(10) 0.57185(10) 0.58044(3) 0.0237(3) Uiso 1.000000 1 R . .
C10 C 0.32029(10) 0.41285(11) 0.62792(3) 0.0220(2) Uani 1.000000 1 . . .
H10a H 0.30810(10) 0.35501(11) 0.64721(3) 0.0264(3) Uiso 1.000000 1 R . .
H10b H 0.40288(10) 0.46674(11) 0.62641(3) 0.0264(3) Uiso 1.000000 1 R . .
C11 C 0.26123(12) 0.47686(13) 0.64094(4) 0.0302(3) Uani 1.000000 1 . . .
H11a H 0.2755(10) 0.5366(8) 0.6226(2) 0.0453(4) Uiso 1.000000 1 GR . .
H11b H 0.17941(18) 0.4241(2) 0.6428(4) 0.0453(4) Uiso 1.000000 1 GR . .
H11c H 0.2908(9) 0.5111(10) 0.66579(18) 0.0453(4) Uiso 1.000000 1 GR . .
C12 C 0.19420(11) 0.23649(10) 0.59104(4) 0.0249(2) Uani 1.000000 1 . . .
H12a H 0.21046(11) 0.19838(10) 0.57008(4) 0.0299(3) Uiso 1.000000 1 R . .
H12b H 0.19937(11) 0.20184(10) 0.61507(4) 0.0299(3) Uiso 1.000000 1 R . .
C13 C 0.07379(11) 0.21428(13) 0.58659(4) 0.0313(3) Uani 1.000000 1 . . .
H13a H 0.0680(3) 0.2498(10) 0.5632(2) 0.0469(4) Uiso 1.000000 1 GR . .
H13b H 0.02112(16) 0.13232(13) 0.5854(4) 0.0469(4) Uiso 1.000000 1 GR . .
H13c H 0.0545(4) 0.2464(10) 0.6083(2) 0.0469(4) Uiso 1.000000 1 GR . .
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.0030380000826
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.215599998832
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390
32.90890 0.250800013542
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.5290002823
'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C5 O1 H1 97.2(17) . .
H1b C1 H1a 107.9 . .
N1 C1 H1a 109.25(5) 2_665 .
N1 C1 H1b 109.25(7) 2_665 .
C2 C1 H1a 109.25(6) . .
C2 C1 H1b 109.25(6) . .
C2 C1 N1 111.82(10) . 2_665
C1 N1 C1 111.14(7) . 3_565
C1 N1 C1 111.14(6) 2_665 3_565
C1 N1 C1 111.14(7) 2_665 .
C3 N2 C2 119.42(11) . .
N2 C2 C1 110.41(10) . .
H2a C2 C1 109.57(6) . .
H2a C2 N2 109.57(6) . .
H2b C2 C1 109.57(6) . .
H2b C2 N2 109.57(7) . .
H2b C2 H2a 108.1 . .
C10 N3 C7 121.53(10) . .
C12 N3 C7 120.54(10) . .
C12 N3 C10 117.77(10) . .
H3 C3 N2 119.23(7) . .
C4 C3 N2 121.55(11) . .
C4 C3 H3 119.23(6) . .
C4 C5 O1 120.95(10) . .
C6 C5 O1 117.92(10) . .
C6 C5 C4 121.12(10) . .
C5 C4 C3 120.80(10) . .
C9 C4 C3 121.86(11) . .
C9 C4 C5 117.33(10) . .
H6 C6 C5 119.43(6) . .
C7 C6 C5 121.14(10) . .
C7 C6 H6 119.43(6) . .
C6 C7 N3 120.83(10) . .
C8 C7 N3 121.33(11) . .
C8 C7 C6 117.81(10) . .
H9 C9 C4 118.93(7) . .
C8 C9 C4 122.14(11) . .
C8 C9 H9 118.93(7) . .
C9 C8 C7 120.34(10) . .
H8 C8 C7 119.83(7) . .
H8 C8 C9 119.83(7) . .
H10a C10 N3 108.74(6) . .
H10b C10 N3 108.74(6) . .
H10b C10 H10a 107.6 . .
C11 C10 N3 114.04(10) . .
C11 C10 H10a 108.74(7) . .
C11 C10 H10b 108.74(7) . .
H11a C11 C10 109.5 . .
H11b C11 C10 109.5 . .
H11b C11 H11a 109.5 . .
H11c C11 C10 109.5 . .
H11c C11 H11a 109.5 . .
H11c C11 H11b 109.5 . .
H12a C12 N3 108.68(7) . .
H12b C12 N3 108.68(7) . .
H12b C12 H12a 107.6 . .
C13 C12 N3 114.30(12) . .
C13 C12 H12a 108.68(8) . .
C13 C12 H12b 108.68(7) . .
H13a C13 C12 109.5 . .
H13b C13 C12 109.5 . .
H13b C13 H13a 109.5 . .
H13c C13 C12 109.5 . .
H13c C13 H13a 109.5 . .
H13c C13 H13b 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 H1 0.876(10) .
O1 C5 1.3511(13) .
C1 H1a 0.9900 .
C1 H1b 0.9900 .
C1 N1 1.4619(12) 2_665
C1 C2 1.5285(18) .
N2 C2 1.4519(15) .
N2 C3 1.2817(17) .
C2 H2a 0.9900 .
C2 H2b 0.9900 .
N3 C7 1.3741(15) .
N3 C10 1.4654(15) .
N3 C12 1.4623(16) .
C3 H3 0.9500 .
C3 C4 1.4479(16) .
C5 C4 1.4116(15) .
C5 C6 1.3897(15) .
C4 C9 1.4071(16) .
C6 H6 0.9500 .
C6 C7 1.4077(15) .
C7 C8 1.4214(16) .
C9 H9 0.9500 .
C9 C8 1.3814(15) .
C8 H8 0.9500 .
C10 H10a 0.9900 .
C10 H10b 0.9900 .
C10 C11 1.5221(18) .
C11 H11a 0.9800 .
C11 H11b 0.9800 .
C11 H11c 0.9800 .
C12 H12a 0.9900 .
C12 H12b 0.9900 .
C12 C13 1.519(2) .
C13 H13a 0.9800 .
C13 H13b 0.9800 .
C13 H13c 0.9800 .
#BEGIN Loops that were not found in dictionaries:
loop_
_restr_distance_atom_site_label_1
_restr_distance_atom_site_label_2
_restr_distance_site_symmetry_2
_restr_distance_target
_restr_distance_target_weight_param
_restr_distance_diff
O1 H1 1 0.8700 0.0100 -0.0058
#END Loops that were not found in dictionaries
