Crystal structure of bis[diaqua(1,10-phenanthroline-κ 2 N, N′)-copper(II)]diphenylphosphopentamolybdate dihydrate, C36H38Cu2Mo5N4O27P2
Li, Dong-Dong; Jiang, Hui; Jia, Bing-Xin; Yuan, Yuan; Shi, Ye-Shun; Ma, Feng-Xia; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 861–862; doi:10.1515/ncrs-2019-0032

data_8105874
_publ_section_title
;
 Crystal structure of bis[diaqua(1,10-phenanthroline-\k 2 N,
 N&#x2032;)-copper(II)]diphenylphosphopentamolybdate dihydrate,
 C36H38Cu2Mo5N4O27P2
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              861
_journal_page_last               862
_journal_paper_doi               10.1515/ncrs-2019-0032
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         'C36 H34 Cu2 Mo5 N4 O25 P2, 2(H2 O)'
_chemical_formula_sum            'C36 H38 Cu2 Mo5 N4 O27 P2'
_chemical_formula_weight         1627.42
_chemical_name_systematic
;         
bis [diaqua (1,10-phenanthroline-<i>\k</i>^2^<i>N</i>,
<i>N'</i> ) -copper(II) ] diphenylphosphopentamolybdate dihydrate, [{Cu(H~2~O)
~2~ (phen) }~2~{(C~6~H~5~PO~3~) ~2~Mo~5~O~15~}]\\cdot2H~2~O
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_cell_angle_alpha                90
_cell_angle_beta                 98.858(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6362(11)
_cell_length_b                   13.2418(9)
_cell_length_c                   23.6641(14)
_cell_measurement_reflns_used    11550
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.0210
_cell_measurement_theta_min      5.0270
_cell_volume                     4841.2(6)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24274
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         4.918
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.278
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.233
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar-type
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4925
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0263
_refine_ls_R_factor_gt           0.0219
_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^)+(0.0185P)^2^+12.8479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0522
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4449
_reflns_number_total             4925
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2019-0032_suppl.cif
_cod_data_source_block           shelx
_cod_database_code               8105874
_shelx_estimated_absorpt_t_max   0.796
_shelx_estimated_absorpt_t_min   0.748
_exptl_absorpt_special_details   bar-type
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O13-O14
 2.61 with sigma of 0.2
3.a Free rotating group:
 O14(H14A,H14B)
3.b Rotating group:
 O12(H12A,H12B), O13(H13A,H13B)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18)
;
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_funding_html
;
;