Crystal structure of poly[aqua-μ2-4,4′-bis(pyrid-4-yl)biphenyl-κ2 N:N′)-μ4-4′-methyl-[1,1′-biphenyl]-3,5-dicarboxylato-κ4 O:O′:O′′:O′′′)manganese(II)], C52H40N2O10Mn2
Chen, Shi-Jun; Li, Shi-Hui; Wang, Wei-Hua; Long, Yong-Fu; Zhang, Wen-Lai; Wang, Tao; Xu, Yan-Li; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 373–375; doi:10.1515/ncrs-2017-0312

data_8105650
_publ_section_title
;
 Crystal structure of
 poly[aqua-\m2-4,4&#x2032;-bis(pyrid-4-yl)biphenyl-\k2
 N:N&#x2032;)-\m4-4&#x2032;-methyl-[1,1&#x2032;-biphenyl]-3,5-dicarboxylato-\k4
 O:O&#x2032;:O&#x2032;&#x2032;:O&#x2032;&#x2032;&#x2032;)manganese(II)],
 C52H40N2O10Mn2
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              373
_journal_page_last               375
_journal_paper_doi               10.1515/ncrs-2017-0312
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety
;
(C52 H38 Mn2 N2 O9), (H2O)
;
_chemical_formula_sum            'C52 H40 Mn2 N2 O10'
_chemical_formula_weight         962.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 92.828(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.6162(4)
_cell_length_b                   11.0217(5)
_cell_length_c                   45.266(2)
_cell_measurement_reflns_used    3738
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1570
_cell_measurement_theta_min      3.6420
_cell_volume                     4293.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1169
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            11721
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.44
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.655
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
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    1.489
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         3974
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0704
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc 
calc w=1/[\s^2^(Fo^2^)+(0.0305P)^2^+2.2189P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                2974
_reflns_number_total             3974
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2017-0312_suppl.cif
_cod_data_source_block           3
_cod_database_code               8105650
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.13