CO<sub>2</sub> activation by permethylpentalene amido zirconium complexes.
Hamilton, Elizabeth A.; Kilpatrick, Alexander F. R.; Turner, Zoë R; Fraser, Duncan A. X.; Buffet, Jean-Charles; O'Hare, Dermot; Dalton transactions (Cambridge, England : 2003) 50 (2021) 4494–4498; doi:10.1039/d1dt00770j

data_7706996
_publ_section_title
;
 CO<sub>2</sub> activation by permethylpentalene amido zirconium
 complexes.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4494
_journal_page_last               4498
_journal_paper_doi               10.1039/d1dt00770j
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C40 H38 N2 O4 Zr'
_chemical_formula_sum            'C40 H38 N2 O4 Zr'
_chemical_formula_weight         701.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2021-03-05 deposited with the CCDC.	2021-03-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.045(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.02400(19)
_cell_length_b                   21.6398(5)
_cell_length_c                   18.9459(5)
_cell_measurement_reflns_used    5678
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      76.0980
_cell_measurement_theta_min      4.6600
_cell_volume                     3679.14(15)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43b (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    "'Superflip (Palatinus and Chapuis, 2007)"
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5035
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.982
_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   -120.00  -6.00   1.00   20.00    --  -41.90 -19.00-120.00  114
  2  \w    -49.00  30.00   1.00   20.00    --  -41.90  37.00  60.00   79
  3  \w     89.00 178.00   1.00   97.50    --  111.00  45.00-180.00   89
  4  \w     41.00  99.00   1.00   97.50    --  111.00 -45.00  90.00   58
  5  \w     40.00  84.00   1.00   97.50    --  111.00 -45.00-150.00   44
  6  \w     87.00 178.00   1.00   97.50    --  111.00  30.00-120.00   91
  7  \w    100.00 177.00   1.00   97.50    --  111.00 111.00  60.00   77
  8  \w     40.00  84.00   1.00   97.50    --  111.00 -45.00   0.00   44
  9  \w     44.00  98.00   1.00   97.50    --  111.00 -45.00  30.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0369068000
_diffrn_orient_matrix_UB_12      -0.0136398000
_diffrn_orient_matrix_UB_13      -0.0797283000
_diffrn_orient_matrix_UB_21      -0.1226933000
_diffrn_orient_matrix_UB_22      -0.0453960000
_diffrn_orient_matrix_UB_23      0.0172545000
_diffrn_orient_matrix_UB_31      -0.1141916000
_diffrn_orient_matrix_UB_32      0.0531362000
_diffrn_orient_matrix_UB_33      -0.0055784000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0597
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14982
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.490
_diffrn_reflns_theta_min         6.408
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.771
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.034
_refine_diff_density_max         2.321
_refine_diff_density_min         -2.195
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         7386
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0747
_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^)+(0.0680P)^2^+24.9216P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1949
_refine_ls_wR_factor_ref         0.1992
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6272
_reflns_number_total             7386
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt00770j2.cif
_cod_data_source_block           eh-082
_cod_depositor_comments
'Adding full bibliography for 7706993--7706996.cif.'
_cod_original_cell_volume        3679.13(16)
_cod_database_code               7706996
_chemical_oxdiff_formula         'C48 H50 N2 O4 Zr1'
_shelx_estimated_absorpt_t_max   0.912
_shelx_estimated_absorpt_t_min   0.732
_exptl_absorpt_special_details   multi-scan
_reflns_odcompleteness_completeness 98.08
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,
 H12C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35),
  C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
;
_shelx_shelxl_version_number     2014/7
_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 1.426
_oxdiff_exptl_absorpt_empirical_full_min 0.796