Synthesis and reactions of a zirconium naphthalene complex bearing a tetraanionic C-capped triaryloxide ligand.
Nakanishi, Yusuke; Ishida, Yutaka; Kawaguchi, Hiroyuki; Dalton transactions (Cambridge, England : 2003) 45 (2016) 15879–15885; doi:10.1039/c6dt01848c

data_7039638
_publ_section_title
;
 Synthesis and reactions of a zirconium naphthalene complex bearing a
 tetraanionic C-capped triaryloxide ligand.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15879
_journal_page_last               15885
_journal_paper_doi               10.1039/c6dt01848c
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C65 H90 K2 O5 Zr, 0.5(C5 H12), 0.5(C4 H8 O)'
_chemical_formula_sum            'C69.5 H100 K2 O5.5 Zr'
_chemical_formula_weight         1192.91
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-05-09 deposited with the CCDC.
2016-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.581(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.405(4)
_cell_length_b                   17.330(3)
_cell_length_c                   35.658(7)
_cell_measurement_reflns_used    18662
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.4778
_cell_measurement_theta_min      3.0034
_cell_volume                     13780(4)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2009)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2009)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2009)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku Saturn724+ CCD'
_diffrn_measurement_method       dtproprofit.ref
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            148879
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.469
_diffrn_reflns_theta_min         2.998
_diffrn_source                   'Rotationg Anode'
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Jacobson, 1998)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_meas      ?
_exptl_crystal_description       Chip
_exptl_crystal_F_000             5112
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         1.484
_refine_diff_density_min         -0.675
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1478
_refine_ls_number_reflns         31474
_refine_ls_number_restraints     670
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0893
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1454P)^2^+35.1542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2401
_refine_ls_wR_factor_ref         0.2563
_reflns_Friedel_coverage         0.000
_reflns_number_gt                26351
_reflns_number_total             31474
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01848c2.cif
_cod_data_source_block           shelx
_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.

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7039635--7039638.cif.
;
_cod_original_cell_volume        13780(5)
_cod_original_formula_sum        'C69.50 H100 K2 O5.50 Zr'
_cod_database_code               7039638
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.950
_shelx_res_checksum              29046
_shelx_fab_checksum              72185