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_7232147
_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         'C34 H32 Mo2 N4 O17, 4(H2O)'
_chemical_formula_sum            'C34 H40 Mo2 N4 O21'
_chemical_formula_weight         1032.58
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-06-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2018-08-01 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                97.117(9)
_cell_angle_beta                 104.178(11)
_cell_angle_gamma                115.420(11)
_cell_formula_units_Z            2
_cell_length_a                   11.6690(15)
_cell_length_b                   13.2521(12)
_cell_length_c                   15.392(2)
_cell_measurement_reflns_used    2373
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.1639
_cell_measurement_theta_min      3.0655
_cell_volume                     2011.7(5)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.1034
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11637
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        62.254
_diffrn_reflns_theta_max         62.254
_diffrn_reflns_theta_min         3.068
_exptl_absorpt_coefficient_mu    5.900
_exptl_absorpt_correction_T_max  0.9431
_exptl_absorpt_correction_T_min  0.5885
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.685
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.444
_refine_diff_density_min         -0.995
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     500
_refine_ls_number_reflns         6264
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.296
_refine_ls_R_factor_all          0.1083
_refine_ls_R_factor_gt           0.0769
_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^)+(0.1315P)^2^+4.9044P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2138
_refine_ls_wR_factor_ref         0.2387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4400
_reflns_number_total             6264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra09134j2.cif
_cod_data_source_block           sad
_cod_original_cell_volume        2011.8(5)
_cod_database_code               7232147
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.590
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C6-C7
 1.5 with sigma of 0.2
 C7-O7 = C7-O6
 1.3 with sigma of 0.2
 O4W-O5
 -4.5 with sigma of 0.2
3. Others
 Fixed 1: DFIX(-4.5)
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C20(H20A,H20B), C22(H22A,H22B),
 C23(H23A,H23B)
4.b Aromatic/amide H refined with riding coordinates:
 C17(H17), C16(H16), C15(H15), C14(H14), C11(H11), C10(H10), C9(H9), C8(H8),
 C34(H34), C33(H33), C32(H32), C31(H31), C28(H28), C27(H27), C26(H26), C25(H25)
;
_olex2_submission_special_instructions 'No special instructions were received'