The (Calix[4]arene)chloromolybdate(IV) Anion [MoCl(Calix)]-: A Convenient Entry into Molybdenum Calix[4]arene Chemistry
Udo Radius; J. Attner; Inorganic Chemistry 43 (2004) 8587–8599; doi:10.1021/ic049155o

data_4312267
_publ_contact_author_address
;Institut f\"ur Anorganische Chemie
Engesserstrasse, Geb\"aude 30.45
D-76128 Karlsruhe
Germany
;
_publ_contact_author_email       radius@aoc1.uni_karlsruhe.de
_publ_contact_author_fax         ' Int + 721 608 8440'
_publ_contact_author_name        'Udo Radius'
_publ_contact_author_phone       'Int + 721 608 8097'
_publ_section_title
;
 The (Calix[4]arene)chloromolybdate(IV) Anion [MoCl(Calix)]-: A Convenient
 Entry into Molybdenum Calix[4]arene Chemistry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8587
_journal_page_last               8599
_journal_paper_doi               10.1021/ic049155o
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C80 H109.5 Mo1.5 N5.5 O6'
_chemical_formula_weight         1388.14
_chemical_name_common
'p-tert.Butylcalix[4]arene nitrido molybdate (VI) Tetra(ethyl)ammonium salt'
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.289(5)
_cell_length_b                   46.879(9)
_cell_length_c                   13.499(2)
_cell_measurement_reflns_used    1587
_cell_measurement_temperature    203(2)
_cell_volume                     15371(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.925
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.0942
_diffrn_reflns_av_sigmaI/netI    0.0578
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            49028
_diffrn_reflns_theta_full        17.17
_diffrn_reflns_theta_max         17.17
_diffrn_reflns_theta_min         1.24
_exptl_absorpt_coefficient_mu    0.941
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.200
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             5912
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.240
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     871
_refine_ls_number_reflns         9509
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.214
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+32.4769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1609
_refine_ls_wR_factor_ref         0.1944
_reflns_number_gt                6379
_reflns_number_total             9509
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic049155osi20040629_063754_1.cif
_cod_data_source_block           compound_6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+32.4769P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1045P)^2^+32.4769P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C80 H109.50 Mo1.50 N5.50 O6'
_cod_database_code               4312267