Chromium Amino-bis(phenolate) Complexes as Catalysts for Ring-Opening Polymerization of Cyclohexene Oxide
Ambrose, Kenson; Murphy, Jennifer N.; Kozak, Christopher M.; Macromolecules 52 (2019) 7403–; doi:10.1021/acs.macromol.9b01381

data_1554182
_publ_section_title
;
 Chromium Amino-bis(phenolate) Complexes as Catalysts for Ring-Opening
 Polymerization of Cyclohexene Oxide
;
_journal_issue                   19
_journal_name_full               Macromolecules
_journal_page_first              7403
_journal_paper_doi               10.1021/acs.macromol.9b01381
_journal_volume                  52
_journal_year                    2019
_chemical_formula_moiety         'C35 H55 Cl2 Cr N2 O2, C H2 Cl2'
_chemical_formula_sum            'C36 H57 Cl4 Cr N2 O2'
_chemical_formula_weight         743.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.725(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5813(4)
_cell_length_b                   10.9133(2)
_cell_length_c                   20.9170(4)
_cell_measurement_reflns_used    14774
_cell_measurement_temperature    200
_cell_measurement_theta_max      29.5920
_cell_measurement_theta_min      1.8060
_cell_volume                     4082.87(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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      200
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -70.00 110.00   0.50   10.00    --   20.00  54.00   0.00  360
  2  \w    -70.00 110.00   0.50   10.00    --   20.00  54.00  90.00  360
  3  \w    -70.00 110.00   0.50   10.00    --   20.00  54.00 180.00  360
  4  \w    -70.00 110.00   0.50   10.00    --   20.00  54.00 270.00  360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0113439000
_diffrn_orient_matrix_UB_12      -0.0245423000
_diffrn_orient_matrix_UB_13      -0.0271491000
_diffrn_orient_matrix_UB_21      0.0377453000
_diffrn_orient_matrix_UB_22      0.0140438000
_diffrn_orient_matrix_UB_23      0.0164310000
_diffrn_orient_matrix_UB_31      0.0043266000
_diffrn_orient_matrix_UB_32      -0.0584988000
_diffrn_orient_matrix_UB_33      0.0153338000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0319
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52554
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.682
_diffrn_reflns_theta_min         2.276
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'greenish pink'
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_description       hexagonal
_exptl_crystal_F_000             1580
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.420
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     435
_refine_ls_number_reflns         7755
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0845P)^2^+3.4163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1618
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6470
_reflns_number_total             7755
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma9b01381_si_002.cif
_cod_data_source_block           mun1133_Compd1
_cod_original_cell_volume        4082.87(14)
_cod_database_code               1554182
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CrC37H57Cl6O2N2
_shelx_estimated_absorpt_t_max   0.894
_shelx_estimated_absorpt_t_min   0.803
_reflns_odcompleteness_completeness 94.15
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.49
_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, All O(H) groups
2. Restrained distances
 O2-H2
 0.87 with sigma of 0.01
 C18-H2
 1.887956 with sigma of 0.02
 Cr1-H2
 2.764089 with sigma of 0.02
 Cl4-C36 \\sim C36-Cl5
 with sigma of 0.02
 C28-C29 \\sim C28-C30 \\sim C29-C30 \\sim C28A-C29A \\sim C28A-C30A \\sim
C29A-C30A
 with sigma of 0.04
 C27-C21 \\sim C27-C28 \\sim C27-C29 \\sim C27-C30 \\sim C27-C28A \\sim
C27-C29A \\sim C27-C30A
 with sigma of 0.02
 C9-C10 \\sim C9-C11 \\sim C10-C11 \\sim C10A-C11A \\sim C10A-C9A \\sim C11A-C9A
 with sigma of 0.04
 C8-C4 \\sim C8-C9 \\sim C8-C10 \\sim C8-C11 \\sim C8-C10A \\sim C8-C11A \\sim
C8-C9A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C29) = Uanis(C30A)
Uanis(C30A) = Uanis(C29)
Uanis(C29A) = Uanis(C28)
Uanis(C30) = Uanis(C28A)
Uanis(C11A) = Uanis(C10)
Uanis(C11) = Uanis(C9A)
Uanis(C9) = Uanis(C10A)
4. Rigid body (RIGU) restrains
 Cl4, C36, Cl5, C36
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29A)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C11A)=Sof(H11D)=Sof(H11E)=
 Sof(H11F)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(2)
 Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C16(H16A,H16B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B)
6.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C28A(H28D,H28E,H28F),
 C29A(H29D,H29E,H29F), C30A(H30D,H30E,H30F), C10A(H10D,H10E,H10F), C11A(H11D,
 H11E,H11F), C9A(H9AA,H9AB,H9AC)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C20(H20), C22(H22)
6.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.174
_oxdiff_exptl_absorpt_empirical_full_min 0.919