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_4349490
_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         'C160 H156 N16 Na4 O8'
_chemical_formula_sum            'C160 H156 N16 Na4 O8'
_chemical_formula_weight         2522.96
_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   mixed
_atom_sites_solution_primary     direct
_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                70.678(3)
_cell_angle_beta                 89.763(4)
_cell_angle_gamma                79.664(4)
_cell_formula_units_Z            2
_cell_length_a                   16.0814(14)
_cell_length_b                   19.4781(16)
_cell_length_c                   25.689(2)
_cell_measurement_reflns_used    17756
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4787
_cell_measurement_theta_min      1.1281
_cell_volume                     7457.0(11)
_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  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 7.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.0272
	          2theta: -20.1580
scan:
	Number of images: 270
	           Slice: -110.0000 - 25.0000
	     Image width: 0.5000
	        Exp time: 7.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 45.0272
	          2theta: -20.1580
scan:
	Number of images: 186
	           Slice: -109.2500 - -16.2500
	     Image width: 0.5000
	        Exp time: 7.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.0272
	          2theta: -20.1580
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            59409
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.199
_diffrn_reflns_theta_max         25.199
_diffrn_reflns_theta_min         1.545
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7390
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.124
_exptl_crystal_description       block
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.450
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1725
_refine_ls_number_reflns         26701
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0898
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1140P)^2^+3.9114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2424
_refine_ls_wR_factor_ref         0.2578
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21759
_reflns_number_total             26701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00155f1.cif
_cod_data_source_block           C7
_cod_database_code               4349490
_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, All O(H) groups
2.a Riding coordinates:
 O1(H1), O4(H4), O8(H8), O5(H5)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C7(H7), C11(H11), C14(H14), C16(H16), C22(H22),
 C23(H23), C26(H26), C27(H27), C31(H31), C34(H34), C36(H36), C42(H42), C43(H43),
  C46(H46), C47(H47), C51(H51), C54(H54), C56(H56), C62(H62), C63(H63),
 C66(H66), C67(H67), C71(H71), C74(H74), C76(H76), C82(H82), C83(H83), C86(H86),
  C87(H87), C91(H91), C94(H94), C96(H96), C102(H102), C103(H103), C106(H106),
 C107(H107), C111(H111), C114(H114), C116(H116), C122(H122), C123(H123),
 C126(H126), C127(H127), C131(H131), C134(H134), C136(H136), C142(H142),
 C143(H143), C146(H146), C147(H147), C151(H151), C154(H154), C156(H156)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C30(H30A,H30B,H30C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C), C50(H50A,H50B,H50C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C70(H70A,H70B,H70C), C78(H78A,H78B,H78C), C79(H79A,H79B,
 H79C), C80(H80A,H80B,H80C), C90(H90A,H90B,H90C), C98(H98A,H98B,H98C), C99(H99A,
 H99B,H99C), C100(H10D,H10E,H10F), C110(H11A,H11B,H11C), C118(H11D,H11E,H11F),
 C119(H11G,H11H,H11I), C120(H12A,H12B,H12C), C130(H13A,H13B,H13C), C138(H13D,
 H13E,H13F), C139(H13G,H13H,H13I), C140(H14A,H14B,H14C), C150(H15A,H15B,H15C),
 C158(H15D,H15E,H15F), C159(H15G,H15H,H15I), C160(H16A,H16B,H16C)
;
_shelx_res_checksum              59504
_shelx_hkl_checksum              3518
_shelx_fab_checksum              7155
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'