NIR-responsive metal-containing polymer hydrogel for light-controlled microvalve
Lin, Xusheng; Xie, Weiwei; Lin, Qin; Cai, Yuanting; Hua, Yuhui; Lin, Jianfeng; He, Guomei; Chen, Jiangxi; Polymer Chemistry 12 (2021) 3375–3382; doi:10.1039/D1PY00404B

data_1562624
_publ_section_title
;
 NIR-responsive metal-containing polymer hydrogel for light-controlled
 microvalve
;
_journal_issue                   23
_journal_name_full               'Polymer Chemistry'
_journal_page_first              3375
_journal_page_last               3382
_journal_paper_doi               10.1039/D1PY00404B
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'C78 H60 N2 O4 Os P3, C H2 Cl2, B F4'
_chemical_formula_sum            'C79 H62 B Cl2 F4 N2 O4 Os P3'
_chemical_formula_weight         1544.12
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-03-23 deposited with the CCDC.	2021-05-17 downloaded from the CCDC.
;
_cell_angle_alpha                99.0300(10)
_cell_angle_beta                 103.602(2)
_cell_angle_gamma                101.623(2)
_cell_formula_units_Z            2
_cell_length_a                   13.0037(3)
_cell_length_b                   13.1533(2)
_cell_length_c                   22.7428(4)
_cell_measurement_reflns_used    27708
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      77.1220
_cell_measurement_theta_min      3.6810
_cell_volume                     3617.03(13)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -65.00  24.00   0.50    0.15    --  -47.45  64.00-133.00  178
  2  \w   -115.00 -84.00   0.50    0.15    --  -47.45 -64.00  90.00   62
  3  \w     50.00 120.00   0.50    0.15    --   47.45  64.00-133.00  140
  4  \w    -16.00  26.00   0.50    0.15    --   47.45 -64.00  90.00   84
  5  \w    -83.00 -58.00   0.50    0.40    --  -86.25  64.00-133.00   50
  6  \w   -130.00 -70.00   0.50    0.40    --  -86.25 -64.00  90.00  120
  7  \w     40.00  66.00   0.50    0.40    --  107.75 -64.00  90.00   52
  8  \w     90.00 178.00   0.50    0.40    --  107.75  64.00-133.00  176
  9  \w   -120.00 -95.00   0.50    0.15    --  -47.45-125.00  30.00   50
 10  \w    -68.00  -7.00   0.50    0.15    --  -47.45  77.00 120.00  122
 11  \w   -120.00 -71.00   0.50    0.15    --  -47.45-125.00-120.00   98
 12  \w   -118.00 -71.00   0.50    0.15    --  -47.45-125.00  60.00   94
 13  \w      0.00  25.00   0.50    0.15    --  -47.45  77.00 120.00   50
 14  \w     49.00  79.00   0.50    0.15    --   47.45-125.00  90.00   60
 15  \w    -46.00 -21.00   0.50    0.40    --  -86.25  19.00-120.00   50
 16  \w    -86.00 -50.00   0.50    0.40    --  -86.25  19.00-120.00   72
 17  \w    -82.00 -13.00   0.50    0.40    --  -86.25 125.00 -60.00  138
 18  \w    -74.00 -29.00   0.50    0.40    --  -86.25 125.00-150.00   90
 19  \w     66.00  92.00   0.50    0.40    --  107.75 -99.00-150.00   52
 20  \w     43.00  69.00   0.50    0.40    --  107.75-125.00 -30.00   52
 21  \w     78.00 104.00   0.50    0.40    --  107.75-125.00 -30.00   52
 22  \w     40.00 109.00   0.50    0.40    --  107.75 -99.00-180.00  138
 23  \w     51.00  98.00   0.50    0.40    --  107.75 -99.00 120.00   94
 24  \w    136.00 177.00   0.50    0.40    --  107.75 125.00  60.00   82
 25  \w     59.00 109.00   0.50    0.40    --  107.75 -99.00   0.00  100
 26  \w     35.00  82.00   0.50    0.40    --  107.75 -99.00 150.00   94
 27  \w     86.00 120.00   0.50    0.40    --  107.75 -37.00-150.00   68
 28  \w     95.00 169.00   0.50    0.40    --  107.75  19.00 -30.00  148
 29  \w     35.00  72.00   0.50    0.40    --  107.75 -37.00-150.00   74
 30  \w     74.00 115.00   0.50    0.40    --  107.75 -37.00-180.00   82
 31  \w     41.00  68.00   0.50    0.40    --  107.75-125.00-150.00   54
 32  \w     85.00 178.00   0.50    0.40    --  107.75  77.00 -30.00  186
 33  \w     39.00  65.00   0.50    0.40    --  107.75-125.00-180.00   52
 34  \w     92.00 117.00   0.50    0.40    --  107.75-125.00-180.00   50
 35  \w    112.00 137.00   0.50    0.40    --  107.75  19.00-150.00   50
 36  \w    143.00 174.00   0.50    0.40    --  107.75  19.00-150.00   62
 37  \w     37.00 107.00   0.50    0.40    --  107.75-125.00  90.00  140
 38  \w     37.00 109.00   0.50    0.40    --  107.75 -99.00-120.00  144
 39  \w     94.00 177.00   0.50    0.40    --  107.75 125.00 150.00  166
 40  \w    101.00 126.00   0.50    0.40    --  107.75 125.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0638334000
_diffrn_orient_matrix_UB_12      0.0488676000
_diffrn_orient_matrix_UB_13      -0.0495285000
_diffrn_orient_matrix_UB_21      0.0948053000
_diffrn_orient_matrix_UB_22      0.1007501000
_diffrn_orient_matrix_UB_23      0.0192327000
_diffrn_orient_matrix_UB_31      0.0526512000
_diffrn_orient_matrix_UB_32      -0.0494990000
_diffrn_orient_matrix_UB_33      -0.0476320000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0823
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43711
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.584
_diffrn_reflns_theta_min         3.512
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.135
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.20457
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'orangish red'
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       plate
_exptl_crystal_F_000             1556
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.672
_refine_diff_density_min         -3.380
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         14760
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0758
_refine_ls_R_factor_gt           0.0680
_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^)+(0.0797P)^2^+38.3350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1716
_refine_ls_wR_factor_ref         0.1825
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13895
_reflns_number_total             14760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1py00404b2.cif
_cod_data_source_block           lqq-20180712-1_sq
_cod_depositor_comments          'Adding full bibliography for 1562624.cif.'
_cod_database_code               1562624
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.628
_shelx_estimated_absorpt_t_min   0.233
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C019(H019)
2.b Secondary CH2 refined with riding coordinates:
 C02P(H02I,H02K)
2.c Aromatic/amide H refined with riding coordinates:
 C00E(H00E), C00J(H00J), C00M(H00M), C00N(H00N), C00O(H00O), C00Q(H00Q),
 C00U(H00U), C00V(H00V), C00W(H00W), C00X(H00X), C00Z(H00Z), C011(H011),
 C013(H013), C015(H015), C016(H016), C01A(H01A), C01B(H01B), C01C(H01C),
 C01F(H01F), C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J), C01K(H01K),
 C01L(H01L), C01N(H01N), C01O(H01O), C01P(H01P), C01Q(H01Q), C01R(H01R),
 C01S(H01S), C01T(H01T), C01U(H01U), C01V(H01V), C01W(H01W), C01X(H01X),
 C01Y(H01Y), C01Z(H01Z), C021(H021), C022(H022), C023(H023), C024(H024),
 C025(H025), C026(H026), C027(H027), C028(H028), C029(H029), C02A(H02A),
 C02B(H02B), C02C(H02C), C02D(H02D), C02E(H02E), C02F(H02F), C02G(H02G),
 C02H(H02H), C02J(H02J), C02L(H02L), C02M(H02M), C02N(H02N)
;
_shelx_res_checksum              26466
_shelx_fab_checksum              40116
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.748
_oxdiff_exptl_absorpt_empirical_full_min 0.427