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_4349495
_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         'C48 H42 Br2 Mg2 N8, 2(C2 H3 N)'
_chemical_formula_sum            'C52 H48 Br2 Mg2 N10'
_chemical_formula_weight         1021.44
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_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            4
_cell_length_a                   17.232(3)
_cell_length_b                   16.286(3)
_cell_length_c                   16.384(3)
_cell_measurement_reflns_used    15268
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4780
_cell_measurement_theta_min      1.2503
_cell_volume                     4598.0(14)
_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: 270.0000
	             XTD: 45.0199
	          2theta: -20.2246
scan:
	Number of images: 240
	           Slice: -80.0000 - 40.0000
	     Image width: 0.5000
	        Exp time: 3.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.0199
	          2theta: -20.2246
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0143
_diffrn_orient_matrix_UB_12      -0.0189
_diffrn_orient_matrix_UB_13      0.0567
_diffrn_orient_matrix_UB_21      -0.0593
_diffrn_orient_matrix_UB_22      0.0061
_diffrn_orient_matrix_UB_23      -0.0129
_diffrn_orient_matrix_UB_31      -0.0016
_diffrn_orient_matrix_UB_32      -0.0549
_diffrn_orient_matrix_UB_33      -0.0187
_diffrn_radiation_detector       CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            30843
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.72
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    1.840
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8034
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.476
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.192
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.012(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         10110
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0469P)^2^+1.5834P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1073
_reflns_number_gt                9493
_reflns_number_total             10110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00177g2.cif
_cod_data_source_block           C1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        4597.9(16)
_cod_database_code               4349495
_diffrn_number_total             5833
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N1AA(H1AA), N5(H5)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C47(H47A,
 H47B), C53(H53A,H53B), C57(H57A,H57B), C62(H62A,H62B), C64(H64A,H64B),
 C67(H67A,H67B)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C17(H17), C23(H23), C26(H26), C27(H27), C30(H30), C32(H32),
 C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C48(H48), C49(H49),
  C50(H50), C54(H54), C56(H56), C63(H63), C68(H68)
2.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C1AA(H1AB,H1AC,H1AD)
;
_olex2_submission_special_instructions 'No special instructions were received'