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_7034094
_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         'C130 H179 Cl N Nb O8, 3.5(C2 H3 N)'
_chemical_formula_sum            'C137 H189.5 Cl N4.5 Nb O8'
_chemical_formula_weight         2155.78
_chemical_name_systematic
; 
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-01-15 deposited with the CCDC.
2015-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.6385(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.358(2)
_cell_length_b                   17.6674(12)
_cell_length_c                   24.5131(17)
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.3
_cell_volume                     13121.0(15)
_computing_cell_refinement
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_data_collection
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_data_reduction
; 
Rigaku CrystalClear-SM Expert 3.1 b27 
;
_computing_molecular_graphics    'Bruker SHEXTL'
_computing_publication_material  'Bruker SHEXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.994
_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_radiation_monochromator  Mirrors
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0958
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            69292
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.323
_diffrn_source                   'Sealed Tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.166
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.699
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.091
_exptl_crystal_description       Block
_exptl_crystal_F_000             4660
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_platon_squeeze_details
; (replace by semicolon in column 1 when used as .sqf) 
TITL CR515 in P2(1)/c 
CELL   30.3580   17.6674   24.5131     90.00     93.64     90.00 
SPGR P21/c 
Q101 0.765 0.819 0.664 !       1.39 eA-3 
C102 1.002 0.468 0.537 !       1.30 eA-3 
Q103 0.723 0.686 0.163 !       1.21 eA-3 
Q104 0.804 0.894 0.177 !       1.08 eA-3 
C105 1.000 1.000 0.000 !       1.06 eA-3 
Q106 0.277 0.187 0.381 !       0.90 eA-3 
Q107 0.304 0.655 0.591 !       0.69 eA-3 
Q108 0.232 0.175 0.384 !       0.67 eA-3 
Q109 0.400 0.580 0.415 !       0.63 eA-3 
Q110 0.461 0.405 0.437 !       0.60 eA-3 
Q111 0.985 0.922 0.174 !       0.60 eA-3 
Q112 0.202 0.754 0.390 !       0.60 eA-3 
Q113 0.788 0.654 0.555 !       0.59 eA-3 
C114 0.399 0.794 0.006 !       0.58 eA-3 
Q115 0.491 0.455 0.530 !       0.57 eA-3 
Q116 0.172 0.433 0.283 !       0.57 eA-3 
Q117 0.209 0.045 0.861 !       0.57 eA-3 
Q118 0.678 0.471-0.003 !       0.55 eA-3 
Q119 0.806 0.099 0.365 !       0.55 eA-3 
Q120 0.819 0.521 0.409 !       0.55 eA-3 
Q121 0.233 0.267 0.779 !       0.54 eA-3 
C122 0.642 0.846 0.368 !       0.54 eA-3 
Q123 0.025 0.418 0.736 !       0.54 eA-3 
Q124 0.771 0.719 0.106 !       0.53 eA-3 
Q125 0.220 0.271 0.817 !       0.53 eA-3 
Q126 0.861 0.074 0.350 !       0.52 eA-3 
Q127 0.743 0.830 0.125 !       0.52 eA-3 
Q128 0.905 0.250 0.694 !       0.51 eA-3 
Q129 0.196 0.833 0.070 !       0.51 eA-3 
Q130 0.196 0.277 0.750 !       0.50 eA-3 
Q131 0.186 0.313 0.409 !       0.50 eA-3 
Q132 0.750 0.671 0.196 !       0.50 eA-3 
;
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.904
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1529
_refine_ls_number_reflns         22952
_refine_ls_number_restraints     308
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1349
_refine_ls_R_factor_gt           0.0720
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0567P)^2^+25.6859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1493
_refine_ls_wR_factor_ref         0.1833
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13966
_reflns_number_total             22952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00272a2.cif
_cod_data_source_block           cr515
_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_original_formula_sum        'C137 H189.50 Cl N4.50 Nb O8'
_cod_database_code               7034094
_shelx_estimated_absorpt_t_min   0.987
_shelx_estimated_absorpt_t_max   0.990
_shelxl_version_number           2014-3
_shelx_res_checksum              56401