Magnesium and aluminum complexes bearing bis(5,6,7-trihydro quinolyl)-fused benzodiazepines for ε-caprolactone polymerization
Rajendran, Natesan Mannangatti; Xi, Yanxia; Zhang, Wenjuan; Braunstein, Pierre; Liang, Tongling; Sun, Wen-Hua; Inorganic Chemistry Frontiers 3 (2016) 1317–; doi:10.1039/C6QI00177G

data_4349494
_publ_section_title
;
 Magnesium and aluminum complexes bearing bis(5,6,7-trihydro
 quinolyl)-fused benzodiazepines for \e-caprolactone polymerization
;
_journal_issue                   10
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1317
_journal_paper_doi               10.1039/C6QI00177G
_journal_volume                  3
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C24 H20 Cl2 N4'
_chemical_formula_sum            'C24 H20 Cl2 N4'
_chemical_formula_weight         435.34
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-05-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-01 deposited with the CCDC.
2016-08-18 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.070(3)
_cell_length_b                   19.070(3)
_cell_length_c                   12.810(3)
_cell_measurement_reflns_used    16028
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4718
_cell_measurement_theta_min      1.5099
_cell_volume                     4658.5(15)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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: 90.0000
	             XTD: 45.0271
	          2theta: -20.0690
scan:
	Number of images: 240
	           Slice: -80.0000 - 40.0000
	     Image width: 0.5000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 45.0271
	          2theta: -20.0690
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0228
_diffrn_orient_matrix_UB_12      -0.0130
_diffrn_orient_matrix_UB_13      -0.0454
_diffrn_orient_matrix_UB_21      0.0469
_diffrn_orient_matrix_UB_22      -0.0122
_diffrn_orient_matrix_UB_23      -0.0201
_diffrn_orient_matrix_UB_31      -0.0084
_diffrn_orient_matrix_UB_32      -0.0734
_diffrn_orient_matrix_UB_33      0.0252
_diffrn_radiation_detector       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31184
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.39
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.0000
_exptl_absorpt_correction_T_min  0.0000
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1808
_platon_squeeze_details
;
;
_refine_diff_density_max         0.342
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5327
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+1.0500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1085
_reflns_number_gt                5257
_reflns_number_total             5327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00177g2.cif
_cod_data_source_block           L3
_cod_original_cell_volume        4658.5(13)
_cod_database_code               4349494
_diffrn_number_total             3083
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2.a Riding coordinates:
 N1(H1)
2.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B), C11(H11A,H11B)
2.c Aromatic/amide H refined with riding coordinates:
 N2(H2), C24(H24), C21(H21), C8(H8), C22(H22), C9(H9), C16(H16), C17(H17),
 C23(H23)
;
_olex2_submission_special_instructions 'No special instructions were received'