Concomitance of octamolybdate isomers in metastable crystal structures isolated using homoleptic Co^II^/Co^III^ complexes as structure-directing templates
Atencio, Reinaldo; Briceño, Alexander; Bruno-Colmenarez, Julia; Silva, Pedro; Rodríguez, Laura; Sosa, Eleida; Limones, Erick; Pacheco, Yesenia; Cáceres, Julio; Vielma, Joel; Acta Crystallographica Section B 77 (2021) 99–114; doi:10.1107/S2052520620015905

data_2108747
_publ_section_title
;
 Concomitance of octamolybdate isomers in metastable crystal structures
 isolated using homoleptic Co^II^/Co^III^ complexes as structure-directing
 templates
;
_journal_coeditor_code           UM5046
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              99
_journal_page_last               114
_journal_paper_doi               10.1107/S2052520620015905
_journal_volume                  77
_journal_year                    2021
_chemical_formula_iupac
'[Co (C10 H8 N2)3]2 [{Mo8 O26}0.5 {Mo8 O26}], 12H2 O'
_chemical_formula_moiety
'2(C30 H24 Co N6 3+), 3(Mo4 O13 2-), 12(H2 O)'
_chemical_formula_sum            'C60 H72 Co2 Mo12 N12 O51'
_chemical_formula_weight         3046.43
_chemical_name_systematic
;
Bis[tris(2,2'-bipyridine)cobaltate(II)] sesqui(octamolydate) dodecahydrate
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-09-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.218(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.151(4)
_cell_length_b                   21.972(6)
_cell_length_c                   37.570(3)
_cell_measurement_reflns_used    17236
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      25.240
_cell_measurement_theta_min      1.853
_cell_volume                     9132(4)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Rigaku AFC-7S/Mercury (2x2 bin mode)'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1384
_diffrn_reflns_av_unetI/netI     0.1365
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            17236
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.152
_diffrn_reflns_theta_min         1.853
_exptl_absorpt_coefficient_mu    2.043
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            'light orange'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_description       needle
_exptl_crystal_F_000             5928
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.842
_refine_diff_density_min         -0.821
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1126
_refine_ls_number_reflns         16166
_refine_ls_number_restraints     522
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1550
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0565P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1245
_refine_ls_wR_factor_ref         0.1584
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7572
_reflns_number_total             16166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            um5046sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 2108746--2108748.cif.'
_cod_database_code               2108747
_cod_database_fobs_code          2108747
_publcif_datablock.id            {c3fdbadd-20e3-4fd4-ba06-4ea0b7be5669}
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.400
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid body (RIGU) restrains
 N11, N21, C11, C21, C31, C41, C51, C61, C71, C81, C91, C101, N31, N41, C111,
 C121, C131, C141, C151, C161, C171, C181, C191, C201, N51, N61, C211, C221,
 C231, C241, C251, C261, C271, C281, C291, C301, N12, N22, C12, C22, C32, C42,
 C52, C62, C72, C82, C92, C102, N32, N42, C112, C122, C132, C142, C152, C162,
 C172, C182, C192, C202, N52, N62, C212, C222, C232, C242, C252, C262, C272,
 C282, C292, C302
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C21(H21), C31(H31), C41(H41), C71(H71), C81(H81), C91(H91),
 C101(H101), C111(H111), C121(H121), C131(H131), C141(H141), C171(H171),
 C181(H181), C191(H191), C201(H201), C211(H211), C221(H221), C231(H231),
 C241(H241), C271(H271), C281(H281), C291(H291), C301(H301), C12(H12), C22(H22),
  C32(H32), C42(H42), C72(H72), C82(H82), C92(H92), C102(H102), C112(H112),
 C122(H122), C132(H132), C142(H142), C172(H172), C182(H182), C192(H192),
 C202(H202), C212(H212), C222(H222), C232(H232), C242(H242), C272(H272),
 C282(H282), C292(H292), C302(H302)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              78260
_shelx_hkl_checksum              86458
_shelx_fab_checksum              2443
_olex2_submission_special_instructions 'No special instructions were received'