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_7034096
_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, 2(C2 H3 N)'
_chemical_formula_sum            'C68 H96 N2 O4'
_chemical_formula_weight         1005.46
_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   mixed
_atom_sites_solution_primary     other
_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                75.412(12)
_cell_angle_beta                 69.309(11)
_cell_angle_gamma                73.026(12)
_cell_formula_units_Z            2
_cell_length_a                   14.6430(10)
_cell_length_b                   15.4125(11)
_cell_length_c                   16.1202(11)
_cell_measurement_reflns_used    21877
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.9
_cell_measurement_theta_min      2.3
_cell_volume                     3209.9(5)
_computing_cell_refinement
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_collection
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_data_reduction
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 20112)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT, (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support MiTeGen
_diffrn_radiation_monochromator  Mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2157
_diffrn_reflns_av_unetI/netI     0.2223
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21642
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        22.500
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_min         2.291
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.113
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1100
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     728
_refine_ls_number_reflns         8056
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.2856
_refine_ls_R_factor_gt           0.1460
_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^)+(0.1940P)^2^+13.0654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3418
_refine_ls_wR_factor_ref         0.4837
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3030
_reflns_number_total             8056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00272a2.cif
_cod_data_source_block           cr521
_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               7034096
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.994
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              9158