Sodium iminoquinolates with cubic and hexagonal prismatic motifs: synthesis, characterization and their catalytic behavior toward the ROP of rac-lactide
Zhang, Qiurui; Zhang, Wenjuan; Wang, Shengdong; Solan, Gregory A.; Liang, Tongling; Rajendran, Natesan Mannangatti; Sun, Wen-Hua; Inorganic Chemistry Frontiers 3 (2016) 1178–; doi:10.1039/C6QI00155F

data_4349487
_publ_section_title
;
 Sodium iminoquinolates with cubic and hexagonal prismatic motifs:
 synthesis, characterization and their catalytic behavior toward the ROP
 of rac-lactide
;
_journal_issue                   9
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1178
_journal_paper_doi               10.1039/C6QI00155F
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'C132 H136.43 N12 Na6 O6, 2(C7 H8)'
_chemical_formula_sum            'C146 H152 N12 Na6 O6'
_chemical_formula_weight         2308.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-07-05 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                100.84(3)
_cell_angle_beta                 105.10(3)
_cell_angle_gamma                115.30(3)
_cell_formula_units_Z            1
_cell_length_a                   14.507(3)
_cell_length_b                   16.694(3)
_cell_length_c                   17.000(3)
_cell_measurement_reflns_used    9668
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4737
_cell_measurement_theta_min      1.3207
_cell_volume                     3376(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.0121
	          2theta: -19.8851
scan:
	Number of images: 346
	           Slice: -110.0000 - 63.0000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.0121
	          2theta: -19.8851
scan:
	Number of images: 330
	           Slice: -106.2500 - 58.7500
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.0121
	          2theta: -19.8851
scan:
	Number of images: 180
	           Slice: -87.5000 - 2.5000
	     Image width: 0.5000
	        Exp time: 10.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 45.0121
	          2theta: -19.8851
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       dtprofit.ref
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0455
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            47372
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.57
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8209
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1226
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.086
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     821
_refine_ls_number_reflns         15399
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0781
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+1.7629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1801
_refine_ls_wR_factor_ref         0.1924
_reflns_number_gt                12581
_reflns_number_total             15399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00155f1.cif
_cod_data_source_block           C3
_cod_original_cell_volume        3375.9(12)
_cod_database_code               4349487
_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
2. Others
 Sof(C44I)=Sof(H44D)=Sof(H44E)=Sof(H44F)=Sof(C43I)=Sof(H43D)=Sof(H43E)=
 Sof(H43F)=1-FVAR(1)
 Sof(H42)=Sof(C43)=Sof(H43A)=Sof(H43B)=Sof(H43C)=Sof(C44)=Sof(H44A)=Sof(H44B)=
 Sof(H44C)=FVAR(1)
 Sof(C19I)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C18)=Sof(H18D)=Sof(H18E)=
 Sof(H18F)=1-FVAR(2)
 Sof(H17)=Sof(C18I)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(H19C)=FVAR(2)
3.a Ternary CH refined with riding coordinates:
 C20(H20), C17(H17), C42(H42), C64(H64), C39(H39), C61(H61)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C32(H32), C30(H30), C54(H54), C46(H46), C12(H12), C2(H2), C29(H29),
 C14(H14), C24(H24), C26(H26), C13(H13), C25(H25), C52(H52), C57(H57), C3(H3),
 C4(H4), C37(H37), C58(H58), C8(H8), C51(H51), C35(H35), C59(H59), C47(H47),
 C7(H7), C36(H36), C48(H48), C72(H72), C68(H68), C69(H69), C70(H70), C71(H71)
3.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C), C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C62(H62A,H62B,H62C), C63(H63A,
 H63B,H63C), C41(H41A,H41B,H41C), C18I(H18A,H18B,H18C), C44(H44A,H44B,H44C),
 C19(H19A,H19B,H19C), C73(H73A,H73B,H73C), C44I(H44D,H44E,H44F), C43I(H43D,H43E,
 H43F), C19I(H19D,H19E,H19F), C18(H18D,H18E,H18F)
;
_olex2_submission_special_instructions 'No special instructions were received'