Tetraphenolate niobium and tantalum complexes for the ring opening polymerization of ε-caprolactone.
Al-Khafaji, Yahya; Sun, Xinsen; Prior, Timothy J.; Elsegood, Mark R. J.; Redshaw, Carl; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12349–12356; doi:10.1039/c5dt00272a

data_7034095
_publ_section_title
;
 Tetraphenolate niobium and tantalum complexes for the ring opening
 polymerization of \e-caprolactone.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12349
_journal_page_last               12356
_journal_paper_doi               10.1039/c5dt00272a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C64 H90 O4'
_chemical_formula_sum            'C64 H90 O4'
_chemical_formula_weight         923.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-01-15 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                68.19(3)
_cell_angle_beta                 83.42(5)
_cell_angle_gamma                69.19(4)
_cell_formula_units_Z            2
_cell_length_a                   11.778(11)
_cell_length_b                   15.190(15)
_cell_length_c                   18.55(2)
_cell_measurement_reflns_used    3614
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.2
_cell_measurement_theta_min      2.1
_cell_volume                     2880(5)
_computing_cell_refinement
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_computing_data_collection
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_computing_data_reduction
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'four-circle \k goniometer'
_diffrn_measurement_device_type  CrystalLogic
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroMesh'
_diffrn_radiation_collimation    'Confocal mirrors'
_diffrn_radiation_monochromator  'double crystal silicon'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6889
_diffrn_reflns_av_R_equivalents  0.1786
_diffrn_reflns_av_unetI/netI     0.1483
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32266
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        22.499
_diffrn_reflns_theta_max         22.499
_diffrn_reflns_theta_min         2.178
_diffrn_source                   'DLS beamline I19'
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
Rigaku CrystalClear-SM Expert 3.1 b26 
;
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_description       needle
_exptl_crystal_F_000             1012
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         8221
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.1921
_refine_ls_R_factor_gt           0.1157
_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^)+(0.1242P)^2^+2.8347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2572
_refine_ls_wR_factor_ref         0.3131
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4391
_reflns_number_total             8221
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00272a2.cif
_cod_data_source_block           cr511
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

 Adding full bibliography for 7034090--7034096.cif.
;
_cod_database_code               7034095
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.994
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              26942