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_4349488
_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         'C172 H132 N8 Na4 O4, 2(C7 H8)'
_chemical_formula_sum            'C186 H148 N8 Na4 O4'
_chemical_formula_weight         2651.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-05-26
_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                90.00
_cell_angle_beta                 109.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   31.790(6)
_cell_length_b                   18.998(4)
_cell_length_c                   30.209(6)
_cell_measurement_reflns_used    23388
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4838
_cell_measurement_theta_min      1.2689
_cell_volume                     17210(7)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.0547
	          2theta: -19.9853
scan:
	Number of images: 358
	           Slice: -110.0000 - 69.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 45.0547
	          2theta: -19.9853
scan:
	Number of images: 332
	           Slice: -110.0000 - 56.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.0547
	          2theta: -19.9853
scan:
	Number of images: 180
	           Slice: -87.5000 - 2.5000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.0547
	          2theta: -19.9853
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0157
_diffrn_orient_matrix_UB_12      0.0169
_diffrn_orient_matrix_UB_13      -0.0240
_diffrn_orient_matrix_UB_21      -0.0454
_diffrn_orient_matrix_UB_22      0.0052
_diffrn_orient_matrix_UB_23      -0.0261
_diffrn_orient_matrix_UB_31      -0.0005
_diffrn_orient_matrix_UB_32      0.0342
_diffrn_orient_matrix_UB_33      0.0076
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0882
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            120753
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.27
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6566
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.023
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5584
_exptl_crystal_size_max          0.419
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.122
_platon_squeeze_details
;

;
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.178
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     913
_refine_ls_number_reflns         19726
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.1340
_refine_ls_R_factor_gt           0.1047
_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^)+(0.0648P)^2^+29.0628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2151
_refine_ls_wR_factor_ref         0.2312
_reflns_number_gt                15823
_reflns_number_total             19726
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00155f1.cif
_cod_data_source_block           C4
_cod_original_cell_volume        17210(6)
_cod_database_code               4349488
_diffrn_number_total             20324
_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:
 C61(H61), C31(H31), C74(H74), C18(H18)
2.b Aromatic/amide H refined with riding coordinates:
 C56(H56), C58(H58), C53(H53), C10(H10), C76(H76), C43(H43), C13(H13),
 C15(H15), C45(H45), C63(H63), C80(H80), C3(H3), C39(H39), C86(H86), C82(H82),
 C69(H69), C46(H46), C4(H4), C67(H67), C73(H73), C66(H66), C33(H33), C72(H72),
 C2(H2), C65(H65), C47(H47), C37(H37), C64(H64), C26(H26), C71(H71), C79(H79),
 C77(H77), C36(H36), C30(H30), C27(H27), C92(H92), C34(H34), C78(H78), C20(H20),
  C70(H70), C40(H40), C42(H42), C8(H8), C85(H85), C28(H28), C41(H41), C88(H88),
 C51(H51), C83(H83), C24(H24), C50(H50), C7(H7), C35(H35), C84(H84), C29(H29),
 C21(H21), C89(H89), C22(H22), C91(H91), C23(H23), C90(H90)
2.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C60(H60A,H60B,H60C), C93(H93A,H93B,H93C)
;
_olex2_submission_special_instructions 'No special instructions were received'