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_4512269
_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         '2 K +,C12 H20 Ni2 O22 2-, 7 H2 O'
_chemical_formula_sum            'C12 H34 K2 Ni2 O29'
_chemical_formula_weight         838.01
_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'
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_cell_angle_beta                 92.119(3)
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_cell_formula_units_Z            4
_cell_length_a                   6.7014(2)
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_cell_measurement_reflns_used    5362
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.76
_cell_volume                     2964.51(15)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
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_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
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_diffrn_measured_fraction_theta_max 0.960
_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  0.0533
_diffrn_reflns_av_unetI/netI     0.0916
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            18233
_diffrn_reflns_point_group_measured_fraction_full 0.984
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.024
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_diffrn_source                   'sealed tube with Enhance optics'
_exptl_absorpt_coefficient_mu    1.665
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
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_refine_ls_extinction_coef       0.0004(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         5224
_refine_ls_number_restraints     1021
_refine_ls_restrained_S_all      0.923
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0609P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3452
_reflns_number_total             5224
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cg5009736_si_001.cif
_cod_data_source_block           jmh88
_cod_depositor_comments
'Adding full bibliography for 4512266--4512273.cif.'
_cod_database_code               4512269
_shelx_estimated_absorpt_t_min   0.732
_shelx_estimated_absorpt_t_max   0.851
_shelxl_version_number           2014-3
_shelx_res_checksum              51474
_shelx_hkl_checksum              96131