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_4349485
_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         'C72 H60 N8 Na4 O4'
_chemical_formula_sum            'C72 H60 N8 Na4 O4'
_chemical_formula_weight         1193.24
_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             2016-05-26
_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                81.79(3)
_cell_angle_beta                 71.41(3)
_cell_angle_gamma                89.01(3)
_cell_formula_units_Z            2
_cell_length_a                   14.787(3)
_cell_length_b                   15.067(3)
_cell_length_c                   18.853(4)
_cell_measurement_reflns_used    12984
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4830
_cell_measurement_theta_min      1.1517
_cell_volume                     3938.6(16)
_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 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 40.0610
	          2theta: -19.9474
scan:
	Number of images: 330
	           Slice: -110.0000 - 55.0000
	     Image width: 0.5000
	        Exp time: 5.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 40.0610
	          2theta: -19.9474
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0431
_diffrn_orient_matrix_UB_12      -0.0569
_diffrn_orient_matrix_UB_13      -0.0016
_diffrn_orient_matrix_UB_21      0.0477
_diffrn_orient_matrix_UB_22      -0.0378
_diffrn_orient_matrix_UB_23      -0.0282
_diffrn_orient_matrix_UB_31      0.0224
_diffrn_orient_matrix_UB_32      0.0043
_diffrn_orient_matrix_UB_33      0.0517
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_unetI/netI     0.1087
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            33902
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.15
_diffrn_source                   'Sealed Tube'
_diffrn_source_current           30.0000
_diffrn_source_power             1.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.006
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     801
_refine_ls_number_reflns         17616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1438
_refine_ls_R_factor_gt           0.0882
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1313P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2331
_refine_ls_wR_factor_ref         0.2651
_reflns_number_gt                9031
_reflns_number_total             17616
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00155f1.cif
_cod_data_source_block           C1
_cod_original_cell_volume        3938.6(14)
_cod_database_code               4349485
_diffrn_number_total             17619
_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 Aromatic/amide H refined with riding coordinates:
 C10(H10), C28(H28), C3(H3), C25(H25), C2(H2), C64(H64), C31(H31), C61(H61),
 C57(H57), C21(H21), C60(H60), C24(H24), C42(H42), C5(H5), C23(H23), C20(H20),
 C59(H59), C6(H6), C13(H13), C39(H39), C7(H7), C15(H15), C41(H41), C56(H56),
 C32(H32), C38(H38), C67(H67), C33(H33), C46(H46), C14(H14), C68(H68), C51(H51),
  C69(H69), C43(H43), C49(H49), C50(H50)
2.b Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C62(H62A,H62B,H62C), C71(H71A,H71B,H71C), C18(H18A,H18B,
 H18C), C53(H53A,H53B,H53C), C72(H72A,H72B,H72C), C36(H36A,H36B,H36C), C54(H54A,
 H54B,H54C)
;
_olex2_submission_special_instructions 'No special instructions were received'