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_2108746
_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          '(N H4) [Co (C10 H8 N2)3] [Mo8 O26], 4H2 O1'
_chemical_formula_moiety
'H4 N +, C30 H24 Co N6 3+, 2(Mo4 O13 2-), 4(H2 O1)'
_chemical_formula_sum            'C30 H36 Co Mo8 N7 O30'
_chemical_formula_weight         1801.11
_chemical_name_systematic
;
Ammonium tris(2,2'-bipyridine)cobaltate(II) octamolybdate tetrahydrate

;
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 107.517(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.270(3)
_cell_length_b                   10.993(2)
_cell_length_c                   23.917(3)
_cell_measurement_reflns_used    8270
_cell_measurement_temperature    298
_cell_measurement_theta_max      25.240
_cell_measurement_theta_min      1.786
_cell_volume                     4831.5(13)
_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
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.971
_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  0.0695
_diffrn_reflns_av_unetI/netI     0.0340
_diffrn_reflns_Laue_measured_fraction_full 0.946
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8653
_diffrn_reflns_point_group_measured_fraction_full 0.946
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.786
_exptl_absorpt_coefficient_mu    2.441
_exptl_absorpt_correction_T_max  0.715
_exptl_absorpt_correction_T_min  0.484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.476
_exptl_crystal_description       plate
_exptl_crystal_F_000             3472
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.789
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.00080(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL2013 (Sheldrick, 2015)'
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     724
_refine_ls_number_reflns         8270
_refine_ls_number_restraints     279
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+6.2337P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0650
_refine_ls_wR_factor_ref         0.0703
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6849
_reflns_number_total             8270
_reflns_threshold_expression     'I > 2\s(I)'
_publcif_datablock.id            {964bb08d-909b-4a13-8d8a-cf85b97eeb49}
_cod_data_source_file            um5046sup1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 2108746--2108748.cif.'
_cod_database_code               2108746
_cod_database_fobs_code          2108746
_shelx_estimated_absorpt_t_max   0.810
_shelx_estimated_absorpt_t_min   0.500
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All N(H,H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O2A \\sim O2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
Uanis(N1A) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
3. Rigid body (RIGU) restrains
 N41, C161, C171, C181, C191, C201, C151, C141, C131, C121, C111, N31, C251,
 N51, C211, C221, C231, C241, C261, N61, C301, C291, C281, C271, C91, C101, N21,
  C61, C71, C81, C51, N11, C11, C21, C31, C41
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O1A)=Sof(H1AE)=Sof(H1AF)=1-FVAR(1)
 Sof(O1)=Sof(H1A)=Sof(H1B)=FVAR(1)
 Sof(O2A)=Sof(H2AA)=Sof(H2AB)=1-FVAR(2)
 Sof(O2)=Sof(H2A)=Sof(H2B)=FVAR(2)
5.a Riding coordinates:
 O2A(H2AA,H2AB)
5.b Free rotating group:
 N1A(H1AA,H1AB,H1AC,H1AD), O1(H1A,H1B), O3(H3A,H3B), O2(H2A,H2B), O1A(H1AE,
 H1AF), O4(H4A,H4B)
5.c 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)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              98906
_shelx_hkl_checksum              61519
_olex2_submission_special_instructions 'No special instructions were received'