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_4347576
_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_formula_moiety
'2(C24 H46 Cl4 In2 N4 O2), 1.94(C7 H6.67), C7 H8'
_chemical_formula_sum            'C68.57 H112.86 Cl8 In4 N8 O4'
_chemical_formula_weight         1856.18
_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
_audit_creation_date             2014-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_cell_angle_alpha                84.491(5)
_cell_angle_beta                 83.099(5)
_cell_angle_gamma                83.917(5)
_cell_formula_units_Z            2
_cell_length_a                   11.307(5)
_cell_length_b                   18.369(5)
_cell_length_c                   22.010(5)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.650
_cell_measurement_theta_min      2.228
_cell_volume                     4497(3)
_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, 2008)'
_computing_structure_solution    'SIR97 (Burla et al., 2007)'
_diffrn_ambient_temperature      90
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            93165
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.053
_diffrn_reflns_theta_min         1.119
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.294
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6316
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0648 before and 0.0514 after correction.
The Ratio of minimum to maximum transmission is 0.8469.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       plates
_exptl_crystal_F_000             1888
_exptl_crystal_recrystallization_method
'grown in toluene under slow evaporation'
_exptl_crystal_size_max          0.93
_exptl_crystal_size_mid          0.81
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.926
_refine_diff_density_min         -1.601
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         23586
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1027
_refine_ls_R_factor_gt           0.0571
_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^)+(0.0434P)^2^+23.6198P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1193
_refine_ls_wR_factor_ref         0.1440
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15406
_reflns_number_total             23586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00358_si_002.cif
_cod_data_source_block           pm138
_cod_database_code               4347576
_shelxl_version_number           2013-4
_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. Restrained distances
 C1I-C1N
 1.54 with sigma of 0.02
 C49-H49A = C49-H49B = C49-H49C = C49-C50
 1.45 with sigma of 0.02
 C1Q-C1Y
 2.51 with sigma of 0.0001
3. Uiso/Uaniso restraints and constraints
Uanis(C1N) \\sim Ueq: with sigma of 0.0005 and sigma for terminal atoms of 0.001
4. Rigid body (RIGU) restrains
 C1N
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
 C1Y, C1P, C1Q, C1R, C1S, C1T, C1O
 with sigma for 1-2 distances of 0.0005 and sigma for 1-3 distances of 0.0005
5. Others
 Sof(C1G)=Sof(H1G)=Sof(C1H)=Sof(H1H)=Sof(C1I)=Sof(C1J)=Sof(H1J)=Sof(C1K)=
 Sof(H1K)=Sof(C1L)=Sof(H1L)=Sof(C1N)=Sof(H1NA)=Sof(H1NB)=Sof(H1NC)=1-FVAR(1)
 Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C1A)=Sof(H1A)=Sof(C1B)=Sof(H1B)=Sof(C1C)=
 Sof(C1D)=Sof(H1D)=Sof(C1E)=Sof(H1E)=Sof(C1F)=Sof(H1F)=Sof(C1M)=Sof(H1MA)=
 Sof(H1MB)=Sof(H1MC)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C14(H14A,H14B), C17(H17A,H17B), C18(H18A,
 H18B), C19(H19A,H19B), C23(H23A,H23B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B), C41(H41A,H41B), C42(H42A,H42B), C44(H44A,H44B), C47(H47A,H47B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C27(H27), C29(H29), C51(H51), C52(H52), C53(H53), C54(H54),
 C55(H55), C1A(H1A), C1B(H1B), C1D(H1D), C1E(H1E), C1F(H1F), C1G(H1G), C1H(H1H),
  C1J(H1J), C1K(H1K), C1L(H1L), C1O(H1O), C1Q(H1Q), C1R(H1R), C1S(H1S), C1T(H1T)
6.c Fitted hexagon refined as free rotating group:
 C1G(C1H,C1I,C1J,C1K,C1L), C1O(C1P,C1Q,C1R,C1S,C1T)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C12(H12A,H12B,H12C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C),
 C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C1M(H1MA,H1MB,H1MC), C1N(H1NA,
 H1NB,H1NC), C1Y(H1YA,H1YB,H1YC)
;
_shelx_res_checksum              7275
_shelx_hkl_checksum              61539
_shelx_fab_checksum              6060
_olex2_exptl_crystal_mounting_method 'mounted in oil'
_olex2_submission_special_instructions 'No special instructions were received'