Structural Variation in Mellitate Complexes of First-Row Transition Metals: What Chance for Design?
Clegg, William; Holcroft, James M.; Crystal Growth & Design 14 (2014) 6282–; doi:10.1021/cg5009736

data_4512266
_publ_section_title
;
 Structural Variation in Mellitate Complexes of First-Row Transition
 Metals: What Chance for Design?
;
_journal_issue                   12
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              6282
_journal_paper_doi               10.1021/cg5009736
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'C12 H24 Co3 O24,6 H2 O'
_chemical_formula_sum            'C12 H36 Co3 O30'
_chemical_formula_weight         837.20
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
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_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_a                   17.0348(11)
_cell_length_b                   8.4649(5)
_cell_length_c                   20.0674(11)
_cell_measurement_reflns_used    2795
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.25
_cell_measurement_theta_min      3.04
_cell_volume                     2893.7(3)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
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_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
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_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0871
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11688
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.291
_diffrn_reflns_theta_min         3.137
_diffrn_source                   'sealed tube with Enhance optics'
_exptl_absorpt_coefficient_mu    1.820
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.85
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.922
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.478
_refine_diff_density_rms         0.116
_refine_ls_extinction_coef       0.00024(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014)'
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         3481
_refine_ls_number_restraints     308
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0116P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0587
_refine_ls_wR_factor_ref         0.0669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2313
_reflns_number_total             3481
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5009736_si_001.cif
_cod_data_source_block           jmh32n
_cod_depositor_comments
'Adding full bibliography for 4512266--4512273.cif.'
_cod_database_code               4512266
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.839
_shelx_estimated_absorpt_t_max   0.931
_shelx_res_checksum              19429
_shelx_hkl_checksum              97341