Copolymerization of CHO/CO<sub>2</sub> catalyzed by a series of aluminum amino-phenolate complexes and insights into structure-activity relationships.
Plommer, Hart; Stein, Laura; Murphy, Jennifer N.; Ikpo, Nduka; Mora-Diez, Nelaine; Kerton, Francesca M.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 6884–6895; doi:10.1039/d0dt00726a

data_7704227
_publ_section_title
;
 Copolymerization of CHO/CO<sub>2</sub> catalyzed by a series of aluminum
 amino-phenolate complexes and insights into structure-activity
 relationships.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6884
_journal_page_last               6895
_journal_paper_doi               10.1039/d0dt00726a
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         '2(C34 H52 Al Cl N2 O2), C7 H7'
_chemical_formula_sum            'C75 H111 Al2 Cl2 N4 O4'
_chemical_formula_weight         1257.53
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-26 deposited with the CCDC.	2020-04-29 downloaded from the CCDC.
;
_cell_angle_alpha                75.708(2)
_cell_angle_beta                 89.494(2)
_cell_angle_gamma                74.480(2)
_cell_formula_units_Z            1
_cell_length_a                   7.7750(2)
_cell_length_b                   11.1513(3)
_cell_length_c                   21.4322(5)
_cell_measurement_reflns_used    9270
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.6110
_cell_measurement_theta_min      2.0010
_cell_volume                     1731.77(8)
_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      100
_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    5.00    --   20.00  54.00   0.00  360
  2  \w    -70.00 110.00   0.50    5.00    --   20.00  54.00  90.00  360
  3  \w    -70.00 110.00   0.50    5.00    --   20.00  54.00 180.00  360
  4  \w    -70.00 110.00   0.50    5.00    --   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      0.0159660000
_diffrn_orient_matrix_UB_12      -0.0115192000
_diffrn_orient_matrix_UB_13      -0.0309201000
_diffrn_orient_matrix_UB_21      -0.0236995000
_diffrn_orient_matrix_UB_22      0.0672689000
_diffrn_orient_matrix_UB_23      -0.0141076000
_diffrn_orient_matrix_UB_31      0.0904523000
_diffrn_orient_matrix_UB_32      0.0000566000
_diffrn_orient_matrix_UB_33      0.0039603000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0403
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            22667
_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         25.681
_diffrn_reflns_theta_min         1.965
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86211
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_description       block
_exptl_crystal_F_000             681
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         6588
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+2.2974P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1499
_refine_ls_wR_factor_ref         0.1563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5743
_reflns_number_total             6588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00726a2.cif
_cod_data_source_block           mun1126
_cod_depositor_comments
'Adding full bibliography for 7704226--7704229.cif.'
_cod_database_code               7704227
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         Al2Cl2C75N4O4H108
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.927
_reflns_odcompleteness_completeness 89.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.43
_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
 H35A-C35 = C35-H35B
 0.98 with sigma of 0.02
 H35C-C35 = C35-H35B
 0.98 with sigma of 0.02
 H35A-C35 = C35-H35C
 0.98 with sigma of 0.02
 H35A-H35B
 1.601 with sigma of 0.04
 H35C-H35B
 1.601 with sigma of 0.04
 H35A-H35C
 1.601 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C35 \\sim C36 \\sim C37 \\sim C38: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C35, C36, C36, C37, C37, C38
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5. Others
 Fixed Sof: C35(0.5) H35A(0.5) H35B(0.5) H35C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C13(H13A,H13B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B),
  C33(H33A,H33B), C34(H34A,H34B)
6.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C15(H15), C17(H17), C37(H37), C38(H38)
6.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C)
;
_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 1.178
_oxdiff_exptl_absorpt_empirical_full_min 0.835