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_4349489
_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         'C138 H150 N12 Na6 O6, 2(C7 H8)'
_chemical_formula_sum            'C152 H166 N12 Na6 O6'
_chemical_formula_weight         2394.91
_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             2016-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-26 deposited with the CCDC.
2016-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                110.08(3)
_cell_angle_beta                 104.88(3)
_cell_angle_gamma                109.92(3)
_cell_formula_units_Z            1
_cell_length_a                   14.410(3)
_cell_length_b                   17.255(3)
_cell_length_c                   17.335(3)
_cell_measurement_reflns_used    8963
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4819
_cell_measurement_theta_min      1.3840
_cell_volume                     3448(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
;
????
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 45.2413
	          2theta: -20.0034
scan:
	Number of images: 324
	           Slice: -110.0000 - 52.0000
	     Image width: 0.5000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.2413
	          2theta: -20.0034
scan:
	Number of images: 318
	           Slice: -110.0000 - 49.0000
	     Image width: 0.5000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.2413
	          2theta: -20.0034
scan:
	Number of images: 224
	           Slice: -109.5000 - 2.5000
	     Image width: 0.5000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.2413
	          2theta: -20.0034
;
_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_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0370
_diffrn_orient_matrix_UB_12      0.0373
_diffrn_orient_matrix_UB_13      -0.0624
_diffrn_orient_matrix_UB_21      0.0145
_diffrn_orient_matrix_UB_22      -0.0378
_diffrn_orient_matrix_UB_23      -0.0574
_diffrn_orient_matrix_UB_31      -0.0387
_diffrn_orient_matrix_UB_32      0.0090
_diffrn_orient_matrix_UB_33      -0.0552
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1162
_diffrn_reflns_av_unetI/netI     0.1089
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41307
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.60
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6865
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1276
_exptl_crystal_size_max          0.191
_exptl_crystal_size_mid          0.116
_exptl_crystal_size_min          0.023
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.260
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     809
_refine_ls_number_reflns         12384
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.260
_refine_ls_R_factor_all          0.1771
_refine_ls_R_factor_gt           0.1390
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0397P)^2^+6.8261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2373
_refine_ls_wR_factor_ref         0.2550
_reflns_number_gt                9182
_reflns_number_total             12384
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00155f1.cif
_cod_data_source_block           C5
_cod_original_cell_volume        3448.3(11)
_cod_database_code               4349489
_diffrn_number_total             15616
_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.a Ternary CH refined with riding coordinates:
 C41(H41), C21(H21), C64(H64), C25(H25), C44(H44), C18(H18), C67(H67)
2.b Aromatic/amide H refined with riding coordinates:
 C37(H37), C38(H38), C15(H15), C14(H14), C39(H39), C48(H48), C54(H54), C2(H2),
 C31(H31), C55(H55), C32(H32), C49(H49), C34(H34), C8(H8), C9(H9), C3(H3),
 C60(H60), C57(H57), C62(H62), C11(H11), C26(H26), C61(H61), C16(H16),
 C106(H106), C102(H102), C103(H103), C104(H104), C105(H105)
2.c Idealised Me refined as rotating group:
 C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C), C45(H45A,H45B,H45C), C22(H22A,H22B,H22C), C20(H20A,H20B,H20C), C23(H23A,
 H23B,H23C), C42(H42A,H42B,H42C), C51(H51A,H51B,H51C), C28(H28A,H28B,H28C),
 C5(H5A,H5B,H5C), C43(H43A,H43B,H43C), C46(H46A,H46B,H46C), C19(H19A,H19B,H19C),
  C100(H10A,H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'