Molybdenum imidazole citrate and bipyridine homocitrate in different oxidation states ‒ balance between coordinated α-hydroxy and α-alkoxy groups
Wang, Si-Yuan; Zhou, Zhao-Hui; RSC Advances 9 (2019) 519–; doi:10.1039/C8RA09134J

data_7232148
_publ_section_title
;
 Molybdenum imidazole citrate and bipyridine homocitrate in different
 oxidation states -- balance between coordinated \a-hydroxy and \a-alkoxy
 groups
;
_journal_issue                   1
_journal_name_full               'RSC Advances'
_journal_page_first              519
_journal_paper_doi               10.1039/C8RA09134J
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C6 H6 Cl Mo O9, H2 O, C8 H20 N'
_chemical_formula_sum            'C14 H28 Cl Mo N O10'
_chemical_formula_weight         501.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-16 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6683(3)
_cell_length_b                   12.0711(3)
_cell_length_c                   22.2111(6)
_cell_measurement_reflns_used    1235
_cell_measurement_temperature    173.00(14)
_cell_measurement_theta_max      24.7620
_cell_measurement_theta_min      3.3700
_cell_volume                     2055.97(11)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XH (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.00(14)
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_details
;
  1 omega -106.00  -38.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.2641 -178.0000  -60.0000 68

  2 omega -105.00  -53.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.2641 -178.0000 -180.0000 52

  3 omega  -80.00  -41.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.2641  -77.0000  150.0000 39
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0210376000
_diffrn_orient_matrix_UB_12      -0.0216695000
_diffrn_orient_matrix_UB_13      -0.0287929000
_diffrn_orient_matrix_UB_21      0.0334984000
_diffrn_orient_matrix_UB_22      -0.0485904000
_diffrn_orient_matrix_UB_23      0.0137156000
_diffrn_orient_matrix_UB_31      -0.0836313000
_diffrn_orient_matrix_UB_32      -0.0248971000
_diffrn_orient_matrix_UB_33      -0.0017262000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0868
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.894
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            6054
_diffrn_reflns_point_group_measured_fraction_full 0.842
_diffrn_reflns_point_group_measured_fraction_max 0.726
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.557
_diffrn_reflns_theta_min         3.228
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99252
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.621
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.779
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.119
_refine_ls_abs_structure_details
;
 Flack x determined using 924 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         4183
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0131P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.432
_reflns_Friedel_fraction_full    0.630
_reflns_Friedel_fraction_max     0.506
_reflns_number_gt                3616
_reflns_number_total             4183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra09134j2.cif
_cod_data_source_block           exp_15245
_cod_database_code               7232148
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.67
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O1W(H1Wa,H1Wb)
2.b Secondary CH2 refined with riding coordinates:
 C3(H3a,H3b), C5(H5a,H5b), C7(H7a,H7b), C11(H11a,H11b), C13(H13a,H13b), C9(H9a,
 H9b)
2.c Idealised Me refined as rotating group:
 C8(H8a,H8b,H8c), C14(H14a,H14b,H14c), C10(H10a,H10b,H10c), C12(H12a,H12b,H12c)
2.d Idealised tetrahedral OH refined as rotating group:
 O5(H5), O7(H7)
;
_olex2_date_sample_data_collection 2016-10-15
_olex2_submission_special_instructions 'No special instructions were received'