Group 4 metal complexes of Trost's semi-crown ligand: synthesis, structural characterization and studies on the ring-opening polymerization of lactides and ε-caprolactone.
Rajashekhar, Bijja; Roymuhury, Sagnik K.; Chakraborty, Debashis; Ramkumar, Venkatachalam; Dalton transactions (Cambridge, England : 2003) 44 (2015) 16280–16293; doi:10.1039/c5dt02267c

data_7035976
_publ_section_title
;
 Group 4 metal complexes of Trost's semi-crown ligand: synthesis,
 structural characterization and studies on the ring-opening
 polymerization of lactides and \e-caprolactone.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16280
_journal_page_last               16293
_journal_paper_doi               10.1039/c5dt02267c
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C86 H88 Hf N4 O6'
_chemical_formula_sum            'C86 H88 Hf N4 O6'
_chemical_formula_weight         1452.09
_chemical_name_systematic        Hf
_chemical_properties_physical    'Air-sensitive, Moisture-sensitive'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-07-06
_audit_creation_method
;
Olex2 1.2-dev
(compiled 2015.06.29 svn.r3191 for OlexSys, GUI svn.r3563)
;
_audit_update_record
;
2015-07-20 deposited with the CCDC.
2015-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1654(6)
_cell_length_b                   20.7645(6)
_cell_length_c                   25.2494(9)
_cell_measurement_temperature    298(2)
_cell_volume                     8999.7(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEXII CCD Area Detector'
_diffrn_measurement_method       ' Phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            27976
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.539
_exptl_absorpt_coefficient_mu    1.209
_exptl_absorpt_correction_T_max  0.794
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5(Bruker AXS.Inc)'
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    1.072
_exptl_crystal_description       Block
_exptl_crystal_F_000             3176
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.489
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 3110 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     440
_refine_ls_number_reflns         7909
_refine_ls_number_restraints     429
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0239
_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^)+(0.0271P)^2^+0.8619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0602
_reflns_Friedel_coverage         0.831
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                7211
_reflns_number_total             7909
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt02267c2.cif
_cod_data_source_block           new_sq
_cod_depositor_comments
'Adding full bibliography for 7035976--7035978.cif.'
_cod_original_formula_sum        'C86 H88 Hf N4 O6 '
_cod_database_code               7035976
_shelx_estimated_absorpt_t_max   0.794
_shelx_estimated_absorpt_t_min   0.677
_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. Rigid body (RIGU) restrains
 C24, C1, C2, C6, O1, C3, C7, C5, C25, Hf1, H3, C4, H7A, H7B, N2, H5, H25A,
 H25B, N1, O3, C43, C8, C11, C26, C29, C30, H43A, H43B, H43C, H8A, H8B, C9, C10,
  H11, C12, H26A, H26B, C27, C28, H29, C31, C37, H9A, H9B, H10A, H10B, C13, C19,
  O2, H27A, H27B, H28A, H28B, C32, C36, C38, C42, C14, C18, C20, H2, H32, C33,
 C35, H36, H38, C39, C41, H42, H14, C15, C17, H18, H20, C21, C23, H24, H33, C34,
  H35, H39, C40, H41, H15, C16, H17, H21, C22, H23, H34, H40, H16, H22
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Ternary CH refined with riding coordinates:
 C11(H11), C29(H29)
3.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20),
 C21(H21), C22(H22), C23(H23), C24(H24), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
3.d Idealised Me refined as rotating group:
 C43(H43A,H43B,H43C)
3.e Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_shelx_res_checksum              79608
_shelx_fab_checksum              27435
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'