Bis(amidinate) ligands in early lanthanide chemistry - synthesis, structures, and hydroamination catalysis.
Kazeminejad, Neda; Munzel, Denise; Gamer, Michael T.; Roesky, Peter W.; Chemical communications (Cambridge, England) 53 (2017) 1060–1063; doi:10.1039/c6cc08958e

data_7119278
_publ_section_title
;
 Bis(amidinate) ligands in early lanthanide chemistry - synthesis,
 structures, and hydroamination catalysis.
;
_journal_issue                   6
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1060
_journal_page_last               1063
_journal_paper_doi               10.1039/c6cc08958e
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C184 H168 Cl4 La4 N16 O8, 9(C7 H8)'
_chemical_formula_sum            'C247 H240 Cl4 La4 N16 O8'
_chemical_formula_weight         4257.98
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-14
_audit_creation_method
;
Olex2 1.2
(compiled 2016.09.09 svn.r3337 for OlexSys, GUI svn.r5227)
;
_audit_update_record
;
2016-12-14 deposited with the CCDC.
2016-12-19 downloaded from the CCDC.
;
_cell_angle_alpha                75.2440(10)
_cell_angle_beta                 83.199(2)
_cell_angle_gamma                82.524(2)
_cell_formula_units_Z            2
_cell_length_a                   21.2533(4)
_cell_length_b                   21.6170(4)
_cell_length_c                   25.3669(5)
_cell_measurement_reflns_used    44264
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      1.22
_cell_volume                     11129.9(4)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2009)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED & LANA, PLATON (A.L.Spek, 2009)'
_computing_molecular_graphics    'Diamond 2/3, Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'MS Word, Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'image plate (34cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE image plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device       'two-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.5mm monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0875
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            188811
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.264
_diffrn_reflns_theta_min         1.221
_diffrn_source                   'sealed tube, 12x0.4mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  0.8152
_exptl_absorpt_correction_T_min  0.2643
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       prism
_exptl_crystal_F_000             4388
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.243
_exptl_crystal_size_min          0.192
_refine_diff_density_max         3.634
_refine_diff_density_min         -1.172
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2379
_refine_ls_number_reflns         188811
_refine_ls_number_restraints     495
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.1508
_refine_ls_R_factor_gt           0.0879
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1505P)^2^+26.1413P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2243
_refine_ls_wR_factor_ref         0.2794
_reflns_Friedel_coverage         0.000
_reflns_number_gt                111081
_reflns_number_total             188811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc08958e2.cif
_cod_data_source_block           compound_1_with_all_solvent_molecules
_cod_depositor_comments
'Adding full bibliography for 7119278--7119283.cif.'
_cod_database_code               7119278
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C234-C235
 1.51 with sigma of 0.02
 C220-C221
 1.51 with sigma of 0.02
 C213-C214
 1.51 with sigma of 0.02
 C227-C228
 1.51 with sigma of 0.02
 C185-C186
 1.51 with sigma of 0.02
 C275-C276
 1.51 with sigma of 0.02
 C282-C283
 1.51 with sigma of 0.02
 C261-C262
 1.51 with sigma of 0.02
 C254-C255
 1.51 with sigma of 0.02
 C199-C200
 1.51 with sigma of 0.02
 C206-C207
 1.51 with sigma of 0.02
 C268-C269
 1.51 with sigma of 0.02
 C242-C243 \\sim C243-C244 \\sim C244-C245 \\sim C245-C246 \\sim C246-C247
\\sim C247-C242
 with sigma of 0.02
 C242-C246 \\sim C242-C244 \\sim C247-C245 \\sim C243-C247 \\sim C244-C246
\\sim C243-C245
 with sigma of 0.04
 C235-C236 \\sim C236-C237 \\sim C239-C240 \\sim C240-C235
 with sigma of 0.02
 C235-C239 \\sim C235-C237 \\sim C236-C240 \\sim C237-C239
 with sigma of 0.04
 C234-C240 \\sim C234-C236
 with sigma of 0.04
 C221-C222 \\sim C222-C223 \\sim C223-C224 \\sim C224-C225 \\sim C225-C226
\\sim C226-C221
 with sigma of 0.02
 C221-C225 \\sim C221-C223 \\sim C226-C224 \\sim C222-C226 \\sim C223-C225
\\sim C222-C224
 with sigma of 0.04
 C220-C226 \\sim C220-C222
 with sigma of 0.04
 C214-C219 \\sim C219-C218 \\sim C218-C217 \\sim C217-C216 \\sim C216-C215
\\sim C215-C214
 with sigma of 0.02
 C214-C216 \\sim C214-C218 \\sim C215-C217 \\sim C219-C215 \\sim C218-C216
\\sim C219-C217
 with sigma of 0.04
 C213-C215 \\sim C213-C219
 with sigma of 0.04
 C228-C229 \\sim C229-C230 \\sim C232-C233 \\sim C233-C228
 with sigma of 0.02
 C228-C232 \\sim C228-C230 \\sim C229-C233 \\sim C230-C232
 with sigma of 0.04
 C227-C233 \\sim C227-C229
 with sigma of 0.04
 C186-C187 \\sim C187-C188 \\sim C190-C191 \\sim C191-C186
 with sigma of 0.02
 C186-C190 \\sim C186-C188 \\sim C187-C191 \\sim C188-C190
 with sigma of 0.04
 C185-C191 \\sim C185-C187
 with sigma of 0.04
 C276-C281 \\sim C281-C280 \\sim C280-C279 \\sim C279-C278 \\sim C278-C277
\\sim C277-C276
 with sigma of 0.02
 C276-C278 \\sim C276-C280 \\sim C277-C279 \\sim C281-C277 \\sim C280-C278
\\sim C281-C279
 with sigma of 0.04
 C275-C277 \\sim C275-C281
 with sigma of 0.04
 C283-C288 \\sim C288-C287 \\sim C287-C286 \\sim C286-C285 \\sim C285-C284
\\sim C284-C283
 with sigma of 0.02
 C283-C285 \\sim C283-C287 \\sim C284-C286 \\sim C288-C284 \\sim C287-C285
\\sim C288-C286
 with sigma of 0.04
 C282-C284 \\sim C282-C288
 with sigma of 0.04
 C262-C263 \\sim C263-C264 \\sim C264-C265 \\sim C265-C266 \\sim C266-C267
\\sim C267-C262
 with sigma of 0.02
 C262-C266 \\sim C262-C264 \\sim C267-C265 \\sim C263-C267 \\sim C264-C266
\\sim C263-C265
 with sigma of 0.04
 C261-C267 \\sim C261-C263
 with sigma of 0.04
 C255-C260 \\sim C260-C259 \\sim C259-C258 \\sim C258-C257 \\sim C257-C256
\\sim C256-C255
 with sigma of 0.02
 C255-C257 \\sim C255-C259 \\sim C256-C258 \\sim C260-C256 \\sim C259-C257
\\sim C260-C258
 with sigma of 0.04
 C254-C256 \\sim C254-C260
 with sigma of 0.04
 C200-C205 \\sim C205-C204 \\sim C202-C201 \\sim C201-C200
 with sigma of 0.02
 C200-C202 \\sim C200-C204 \\sim C205-C201 \\sim C204-C202
 with sigma of 0.04
 C199-C201 \\sim C199-C205
 with sigma of 0.04
 C207-C212 \\sim C212-C211 \\sim C209-C208 \\sim C208-C207
 with sigma of 0.02
 C207-C209 \\sim C207-C211 \\sim C212-C208 \\sim C211-C209
 with sigma of 0.04
 C206-C208 \\sim C206-C212
 with sigma of 0.04
 C269-C270 \\sim C270-C271 \\sim C271-C272 \\sim C272-C273 \\sim C273-C274
\\sim C274-C269
 with sigma of 0.02
 C269-C273 \\sim C269-C271 \\sim C274-C272 \\sim C270-C274 \\sim C271-C273
\\sim C270-C272
 with sigma of 0.04
 C268-C274 \\sim C268-C270
 with sigma of 0.04
3. Restrained planarity
 C243, C245, C242, C244, C246, C247
 with sigma of 0.1
 C239, C237, C235, C234, C236, C240
 with sigma of 0.1
 C220, C221, C222, C223, C224, C225, C226
 with sigma of 0.1
 C213, C216, C217, C218, C219, C214, C215
 with sigma of 0.1
 C229, C233, C228, C230, C232, C227
 with sigma of 0.1
 C185, C186, C187, C188, C190, C191
 with sigma of 0.1
 C275, C276, C277, C278, C279, C280, C281
 with sigma of 0.1
 C282, C283, C284, C285, C286, C287, C288
 with sigma of 0.1
 C261, C262, C263, C264, C265, C266, C267
 with sigma of 0.1
 C254, C255, C256, C257, C258, C259, C260
 with sigma of 0.1
 C199, C200, C201, C202, C204, C205
 with sigma of 0.1
 C206, C207, C208, C209, C211, C212
 with sigma of 0.1
 C268, C269, C270, C271, C272, C273, C274
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C243 \\sim C245 \\sim C242 \\sim C244 \\sim C246 \\sim C247: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C239 \\sim C237 \\sim C235 \\sim C234 \\sim C236 \\sim C240: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C220 \\sim C221 \\sim C222 \\sim C223 \\sim C224 \\sim C225 \\sim C226: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C213 \\sim C216 \\sim C217 \\sim C218 \\sim C219 \\sim C214 \\sim C215: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C229 \\sim C233 \\sim C228 \\sim C230 \\sim C232 \\sim C227: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C185 \\sim C186 \\sim C187 \\sim C188 \\sim C190 \\sim C191: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C275 \\sim C276 \\sim C277 \\sim C278 \\sim C279 \\sim C280 \\sim C281: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C282 \\sim C283 \\sim C284 \\sim C285 \\sim C286 \\sim C287 \\sim C288: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C261 \\sim C262 \\sim C263 \\sim C264 \\sim C265 \\sim C266 \\sim C267: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C254 \\sim C255 \\sim C256 \\sim C257 \\sim C258 \\sim C259 \\sim C260: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C199 \\sim C200 \\sim C201 \\sim C202 \\sim C204 \\sim C205: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C206 \\sim C207 \\sim C208 \\sim C209 \\sim C211 \\sim C212: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C268 \\sim C269 \\sim C270 \\sim C271 \\sim C272 \\sim C273 \\sim C274: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 C243, C245, C242, C244, C246, C247
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C239, C237, C235, C234, C236, C240
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C220, C221, C222, C223, C224, C225, C226
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C213, C216, C217, C218, C219, C214, C215
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C229, C233, C228, C230, C232, C227
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C185, C186, C187, C188, C190, C191
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C275, C276, C277, C278, C279, C280, C281
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C282, C283, C284, C285, C286, C287, C288
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C261, C262, C263, C264, C265, C266, C267
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C254, C255, C256, C257, C258, C259, C260
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C199, C200, C201, C202, C204, C205
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C206, C207, C208, C209, C211, C212
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C173, C176, C250, C251
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C173, C176, C175, C174
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C181, C253, C252, C182
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C268, C269, C270, C271, C272, C273, C274
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H16G(0.66667) H16H(0.66667) H16I(0.33333) H16J(0.33333)
 H17A(0.66667) H17B(0.66667) H17C(0.33333) H17D(0.33333) H17E(0.66667)
 H17F(0.66667) H17G(0.33333) H17H(0.33333) H17K(0.33333) H17L(0.33333)
 H17I(0.66667) H17J(0.66667) H18E(0.5) H18F(0.5) H18C(0.5) H18D(0.5) H25C(0.5)
 H25D(0.5) H25A(0.5) H25B(0.5) C248(0.33333) H24A(0.33333) H24B(0.33333)
 C249(0.33333) H24C(0.33333) H24D(0.33333) C250(0.33333) H25E(0.33333)
 H25F(0.33333) C251(0.33333) H25G(0.33333) H25H(0.33333) C252(0.5) H25I(0.5)
 H25J(0.5) C261(0.5) H26A(0.5) H26B(0.5) H26C(0.5) C262(0.5) C263(0.5)
 H263(0.5) C264(0.5) H264(0.5) C265(0.5) H265(0.5) C266(0.5) H266(0.5)
 C267(0.5) H267(0.5) C275(0.33333) H27A(0.33333) H27B(0.33333) H27C(0.33333)
 C276(0.33333) C277(0.33333) H277(0.33333) C278(0.33333) H278(0.33333)
 C279(0.33333) H279(0.33333) C280(0.33333) H280(0.33333) C281(0.33333)
 H281(0.33333) C282(0.33333) H28D(0.33333) H28E(0.33333) H28F(0.33333)
 C283(0.33333) C284(0.33333) H284(0.33333) C285(0.33333) H285(0.33333)
 C286(0.33333) H286(0.33333) C287(0.33333) H287(0.33333) C288(0.33333)
 H288(0.33333) C268(0.33333) H26D(0.33333) H26E(0.33333) H26F(0.33333)
 C269(0.33333) C270(0.33333) H270(0.33333) C271(0.33333) H271(0.33333)
 C272(0.33333) H272(0.33333) C273(0.33333) H273(0.33333) C274(0.33333)
 H274(0.33333) C254(0.5) H25K(0.5) H25L(0.5) H25M(0.5) C255(0.5) C256(0.5)
 H256(0.5) C257(0.5) H257(0.5) C258(0.5) H258(0.5) C259(0.5) H259(0.5)
 C260(0.5) H260(0.5) C213(0.5) H21D(0.5) H21E(0.5) H21F(0.5) C239(0.66667)
 H239(0.66667) C175(0.66667) H17S(0.66667) H17T(0.66667) C170(0.66667)
 H17U(0.66667) H17V(0.66667) C243(0.66667) H243(0.66667) C174(0.66667)
 H17W(0.66667) H17X(0.66667) C237(0.66667) H237(0.66667) C241(0.66667)
 H24E(0.66667) H24F(0.66667) H24G(0.66667) C231(0.66667) H231(0.66667)
 C232(0.66667) H232(0.66667) C233(0.66667) H233(0.66667) C228(0.66667)
 C229(0.66667) H229(0.66667) C230(0.66667) H230(0.66667) C245(0.66667)
 H245(0.66667) C182(0.5) H18I(0.5) H18J(0.5) C235(0.66667) C171(0.66667)
 H17Y(0.66667) H(0.66667) C216(0.5) H216(0.5) C217(0.5) H217(0.5) C234(0.66667)
 H23A(0.66667) H23B(0.66667) H23C(0.66667) C218(0.5) H218(0.5) C236(0.66667)
 H236(0.66667) C219(0.5) H219(0.5) C238(0.66667) H238(0.66667) C220(0.5)
 H22D(0.5) H22E(0.5) H22F(0.5) C240(0.66667) H240(0.66667) C221(0.5)
 C242(0.66667) C222(0.5) H222(0.5) C244(0.66667) H244(0.66667) C223(0.5)
 H223(0.5) C246(0.66667) H246(0.66667) C224(0.5) H224(0.5) C214(0.5) C225(0.5)
 H225(0.5) C215(0.5) H215(0.5) C226(0.5) H226(0.5) C227(0.66667) H22A(0.66667)
 H22B(0.66667) H22C(0.66667) C247(0.66667) H247(0.66667)
7.a Secondary CH2 refined with riding coordinates:
 C169(H16G,H16H), C169(H16I,H16J), C172(H17A,H17B), C172(H17C,H17D), C173(H17E,
 H17F), C173(H17G,H17H), C176(H17K,H17L), C176(H17I,H17J), C177(H17M,H17N),
 C178(H17O,H17P), C179(H17Q,H17R), C180(H18A,H18B), C181(H18E,H18F), C181(H18C,
 H18D), C184(H18G,H18H), C253(H25C,H25D), C253(H25A,H25B), C248(H24A,H24B),
 C249(H24C,H24D), C250(H25E,H25F), C251(H25G,H25H), C252(H25I,H25J), C175(H17S,
 H17T), C170(H17U,H17V), C174(H17W,H17X), C182(H18I,H18J), C171(H17Y,H)
7.b Me refined with riding coordinates:
 C261(H26A,H26B,H26C), C282(H28D,H28E,H28F), C268(H26D,H26E,H26F), C206(H20A,
 H20B,H20C), C254(H25K,H25L,H25M), C213(H21D,H21E,H21F), C234(H23A,H23B,H23C),
 C220(H22D,H22E,H22F), C227(H22A,H22B,H22C)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C10(H10), C11(H11), C12(H12), C16(H16), C17(H17),
 C19(H19), C20(H20), C23(H23), C24(H24), C26(H26), C27(H27), C30(H30), C31(H31),
  C33(H33), C34(H34), C37(H37), C38(H38), C40(H40), C41(H41), C45(H45),
 C46(H46), C47(H47), C52(H52), C53(H53), C54(H54), C58(H58), C59(H59), C61(H61),
  C62(H62), C65(H65), C66(H66), C68(H68), C69(H69), C72(H72), C73(H73),
 C75(H75), C76(H76), C79(H79), C80(H80), C82(H82), C83(H83), C87(H87), C88(H88),
  C89(H89), C94(H94), C95(H95), C96(H96), C100(H100), C101(H101), C103(H103),
 C104(H104), C107(H107), C108(H108), C110(H110), C111(H111), C114(H114),
 C115(H115), C117(H117), C118(H118), C121(H121), C122(H122), C124(H124),
 C125(H125), C129(H129), C130(H130), C131(H131), C136(H136), C137(H137),
 C138(H138), C142(H142), C143(H143), C145(H145), C146(H146), C149(H149),
 C150(H150), C152(H152), C153(H153), C156(H156), C157(H157), C159(H159),
 C160(H160), C163(H163), C164(H164), C166(H166), C167(H167), C263(H263),
 C264(H264), C265(H265), C266(H266), C267(H267), C277(H277), C278(H278),
 C279(H279), C280(H280), C281(H281), C187(H187), C188(H188), C189(H189),
 C190(H190), C191(H191), C284(H284), C285(H285), C286(H286), C287(H287),
 C288(H288), C194(H194), C195(H195), C196(H196), C197(H197), C198(H198),
 C270(H270), C271(H271), C272(H272), C273(H273), C274(H274), C201(H201),
 C202(H202), C203(H203), C204(H204), C205(H205), C208(H208), C209(H209),
 C210(H210), C211(H211), C212(H212), C256(H256), C257(H257), C258(H258),
 C259(H259), C260(H260), C239(H239), C243(H243), C237(H237), C231(H231),
 C232(H232), C233(H233), C229(H229), C230(H230), C245(H245), C216(H216),
 C217(H217), C218(H218), C236(H236), C219(H219), C238(H238), C240(H240),
 C222(H222), C244(H244), C223(H223), C246(H246), C224(H224), C225(H225),
 C215(H215), C226(H226), C247(H247)
7.d Fitted hexagon refined as free rotating group:
 C269(C270,C271,C272,C273,C274), C231(C232,C233,C228,C229,C230)
7.e Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C35(H35A,H35B,H35C), C42(H42A,H42B,
 H42C), C63(H63A,H63B,H63C), C70(H70A,H70B,H70C), C77(H77A,H77B,H77C), C84(H84A,
 H84B,H84C), C105(H10A,H10B,H10C), C112(H11A,H11B,H11C), C119(H11D,H11E,H11F),
 C126(H12A,H12B,H12C), C147(H14A,H14B,H14C), C154(H15A,H15B,H15C), C161(H16A,
 H16B,H16C), C168(H16D,H16E,H16F), C275(H27A,H27B,H27C), C185(H18K,H18L,H18M),
 C192(H19A,H19B,H19C), C199(H19D,H19E,H19F), C241(H24E,H24F,H24G)
;
_shelx_res_checksum              28475
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'