Mechanistic Study of Isotactic Poly(propylene oxide) Synthesis using a Tethered Bimetallic Chromium Salen Catalyst
Lipinski, Bryce M.; Walker, Katherine L.; Clayman, Naomi E.; Morris, Lilliana S.; Jugovic, Timothy M. E.; Roessler, Allison G.; Getzler, Yutan D. Y. L.; MacMillan, Samantha N.; Zare, Richard N.; Zimmerman, Paul M.; Waymouth, Robert M.; Coates, Geoffrey W.; ACS Catalysis  (2020) 8960–8967; doi:10.1021/acscatal.0c02135

data_4517879
_publ_section_title
;
 Mechanistic Study of Isotactic Poly(propylene oxide) Synthesis using a
 Tethered Bimetallic Chromium Salen Catalyst
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              8960
_journal_page_last               8967
_journal_paper_doi               10.1021/acscatal.0c02135
_journal_year                    2020
_chemical_formula_moiety         'C74 H108 Cl Cr2 N5 O5, 0.5[C2H3N]'
_chemical_formula_sum            'C75 H109.5 Cl Cr2 N5.5 O5'
_chemical_formula_weight         1307.62
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0512(8)
_cell_length_b                   20.0506(9)
_cell_length_c                   22.7296(10)
_cell_measurement_reflns_used    21334
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.71
_cell_measurement_theta_min      1.35
_cell_volume                     7770.9(6)
_computing_cell_refinement       'SAINT V5.00 (?, 2016)'
_computing_data_reduction        'SAINT V5.00 (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            63537
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.354
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_T_min  0.594024
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SAD V2.01 (?, 2016) was used for absorption correction. R(int) was 0.0689 before and 0.0484 after correction. The Ratio of minimum to maximum transmission is 0.5940. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.118
_exptl_crystal_description       block
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.9821
_exptl_transmission_factor_min   0.594024
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 4792 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         15881
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0465P)^2^+1.9053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.836
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                12970
_reflns_number_total             15881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c02135_si_001.cif
_cod_data_source_block           m
_cod_depositor_comments          'Adding full bibliography for 4517879.cif.'
_cod_original_cell_volume        7771.0(6)
_cod_database_code               4517879
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.982
_shelx_estimated_absorpt_t_min   0.948
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O5-H5
 0.84 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
4.a Ternary CH refined with riding coordinates:
 C31(H31), C32(H32), C67(H67), C68(H68)
4.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C69(H69A,
 H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B)
4.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C5(H5A), C16(H16), C20(H20), C22(H22), C37(H37), C41(H41),
 C43(H43), C52(H52), C54(H54), C56(H56)
4.d Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C24(H24A,H24B,H24C), C25(H25A,
 H25B,H25C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C47(H47A,H47B,
 H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C60(H60A,
 H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C64(H64A,H64B,H64C),
 C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C74(H74A,H74B,H74C)
;
_shelx_res_checksum              80624
_shelx_hkl_checksum              63869
_shelx_fab_checksum              13215
_olex2_submission_special_instructions 'No special instructions were received'