Dinucleating Ligand Platforms Supporting Indium and Zinc Catalysts for Cyclic Ester Polymerization.
Kremer, Alexandre B.; Osten, Kimberly M.; Yu, Insun; Ebrahimi, Tannaz; Aluthge, Dinesh C.; Mehrkhodavandi, Parisa; Inorganic chemistry 55 (2016) 5365–5374; doi:10.1021/acs.inorgchem.6b00358

data_4347578
_publ_section_title
;
 Dinucleating Ligand Platforms Supporting Indium and Zinc Catalysts for
 Cyclic Ester Polymerization.
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5365
_journal_page_last               5374
_journal_paper_doi               10.1021/acs.inorgchem.6b00358
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C25 H39 Cl3 N4 O Zn2'
_chemical_formula_sum            'C25 H39 Cl3 N4 O Zn2'
_chemical_formula_weight         648.69
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.1516(11)
_cell_length_b                   11.3564(11)
_cell_length_c                   45.652(4)
_cell_measurement_reflns_used    9839
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      24.96
_cell_measurement_theta_min      2.24
_cell_volume                     5781.5(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0984
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            10348
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.404
_diffrn_reflns_theta_max         25.404
_diffrn_reflns_theta_min         1.784
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.962
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0829 before and 0.0617 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0863 before and 0.0650 after correction.
 The Ratio of minimum to maximum transmission is 0.83.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 84603 reflections, Rint = 0.0743
 (44125 with I > 3sig(I), Rint = 0.0546)
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_description       needle
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Flack x determined using 3135 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         10348
_refine_ls_number_restraints     708
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0514
_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^)+(0.0196P)^2^+14.3545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0865
_reflns_Friedel_coverage         0.761
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.952
_reflns_number_gt                8597
_reflns_number_total             10348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00358_si_002.cif
_cod_data_source_block           pm155
_cod_original_cell_volume        5781.5(10)
_cod_database_code               4347578
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.376
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C5(H5), C6(H6), C18(H18), C23(H23), C5A(H5A), C6A(H6A), C18A(H18A), C23A(H23A)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C19(H19A,H19B), C20(H20A,
 H20B), C21(H21A,H21B), C22(H22A,H22B), C1A(H1AA,H1AB), C2A(H2AA,H2AB),
 C3A(H3AA,H3AB), C4A(H4AA,H4AB), C19A(H19C,H19D), C20A(H20C,H20D), C21A(H21C,
 H21D), C22A(H22C,H22D)
3.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C11(H11), C14(H14), C17(H17), C9A(H9A), C11A(H11A), C14A(H14A),
 C17A(H17A)
3.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C24(H24A,H24B,H24C),
 C25(H25A,H25B,H25C), C7A(H7AA,H7AB,H7AC), C8A(H8AA,H8AB,H8AC), C13A(H13D,H13E,
 H13F), C24A(H24D,H24E,H24F), C25A(H25D,H25E,H25F)
;
_shelx_res_checksum              45147
_shelx_hkl_checksum              43047
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'